total synthesis ii strike.docx

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\viewkind4\uc1\pard\lang3082\f0\fs24 TABLE OF CONTENTS

\par DISCLAIMER

\par WARNING! This book is intended for informational purposes only!

\par It is currently illegal to attempt almost any procedure depicted in

INTRODUCTION .................................................................. 5

\par this book. This book does not cendcne ner imply that any proce- EcsTAsY &

AMPHETAMINES ........................................... 7

\par dure lieted herein be deed by the reeder \'a4r enyene else fer thel wi-IERE TO

suv .................................................................. 9

\par meller- Even ll llle eliemlelrv were lege! Slrlke Wellld nel edvlee wi-in TO

Buv ................................................................., 14

\par a"ll\'b0"\'80 *\'b0 \ldblquote >\rquote these l\'b0'\'b0\'b0\'80d"'\'80S *****955 lllel here 6

**\lquote\'b0'\'b0ll9ll \'a4"\'b7 i-iow TO MAKE .. ................... . ..... . .... .. .................... ..18

\par derstanding of chemistry, chemical reactions and methodology. ME.|.H0d\'b0|\'b0gy ' ' " " " '

24

\par gr\'80atha'm\lquote V Pi-iENYLAcEToN'E\'a7'xxIii:3;;;:;;;:::;;iijzizicxziiiii2::;:;;;:;;;:;;:52

\par METHOD #1 .................................................................. 53

\par Copyright @1999 by Strike All righig reserved#2 ..................................................................

\par METHOD #3 .................................................................. 75

\par METHOD #4 .................................................................. 82

\par Panda Ink METHOD #5 .................................................................. BB

\par 2211 NW Military Hwy, Ste. 116 METHOD #6 ..................................................................

93

\par PMB# 115 METHOD #7 .................................................................. 93

\par San Antonio, TX 78213 METHOD #8 .................................................................. 94

\par METHOD #9 .................................................................. 95

\par AMPHETAMIES 8. METHAMPHETAMINES FROM

\par r PHENYLACETONES ......................................................... 97

\par METHOD #1 .................................................................. 98

\par METHOD #2 ,,,...lll..........,............................................ 100

\par METHOD #3 ................................................................ 103


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\par METHOD #4 ................................................................ 104

\par METHOD #5 ...................l............................................ 108

\par METHOD #6 ......................................................,......... 116

\par METHOD #7 ................................................................ 117

\par METHOD #8 .................................................,.............. 117

\par METHOD #9 ................................................................ 120

\par METHOD #10 .............................................................. 122.

\par B-NITROPROPENES .......................................................

\par METHOD #1 ................................................................

\par METHOD #2 ................................................................ 131

\par -2- -3-

\par

\par METHOD #3 ................................................................ 132

\par AMPHETAMINES FROM B-NITROPROPENES .............. 137 |N'|'RQDUc'|'|QN

\par METHOD #1 ................................................................ 138

\par METHOD #2 ................................................................ 139 You have just purchased or

Stolen the most Comprehensive and

\par METHOD #3 ........................................................... . .... 139 detailed book on the

underground production of ecstasy, metham-

\par METHOD #4 ................................................................ 140 phetamine and psychedelic

amphetamines ever published Strike

\par METHOD #5 .......................................... . ..................... 141 (your host) is an ecstasy and

amphetamine chemist from Texas

\par BROMOSAF ROLE & PHENYLlSOPROPYLBROMlDE.. 142 who used to be very

frustrated with the lack of common-sense in-

\par METHOD #1 ................................................................ 145 formation about the produollon

of amphetamines. Strike remedied

\par METHOD #2

________________________________________________________________ 145 this for

Strike and now Strike is gonna remedy it for you, too. This

\par METHOD #3 ...................................................,..,,,.,__,,_ 148 book is oeoked_witn_tne

latest street jnethods for making am.

\par AMPHETAMINES & ME-I-HAMPHETAMINES FROM phetemines - wntten in plain

English with the detail that no other


3/246

\par BRoM0sAr=Roi.E & Pi-iENYt.ls0PR0PYLBR0Ml\'a4E.. 152

b\'b0\'b0*\lquote \'b0a" \'b0""'\'b7

\par METHOD #1 ................................................................ 152 Pius, this edition of -i-mai

Synthesis marks the first Si/Sr C0iiabOia_

\par METHOD #2 ,........................ . .................................. ,...156 tion Of the ch\'80mioa|

undorground_ Throughout tho book you will

\par METHAMPHETAMINES FROM AMPHETAMINES -\'b7\'b7\'b7\'b7\'b7--- 159 find

recipes, secrets and discussions contributed by the worlds

\par METHOD #1 ................................................ . ............... 159 leading underground chemists.

They have Shared their knowledge

\par METHOD #2 ................................................................ 159 so that you may get the best

education availab|o_ So gnjoyi

\par METHOD #3 ................................................................ 160

\par ADVANCED SHRIMP PREPARATION TECHNOLOGY. 161

\par RHODlUM\rquote S CHAPTER ................................................... 164

\par PROMISING THEORETICAL METHODS ........................ 182

\par BUILD FROM SCRATCH ..,..........................................,... 205

\par PYROCATECHOL, GUAIACOL, PHENOL &

\par SALICYLALDEHYDE ........................................,.............. 208

\par METHYLENATION ........................................................... 214

\par BROMINATION OF 1,3-BENZODOIXOLE ...................... 222

\par THE BIG CHAPTER ......................................................... 232

\par THANK YOU SIR MAY I HAVE ANOTHER? .................. 240

\par CRYSTALLIZATION ........................................................ 247

\par CHEMICALS .................................................................... 252

\par REFERENCES ................................................................. 285

\par EPILOGUE ....................................................................... 291

\par . - 4 - - 5 -

\par

\par DISCLAIMER ECSTASY & AMPHETAMINES

\par WARNING! This book is intended for informational purposes only!

\par It is currently illegal to attempt almost any procedure depicted in


4/246

\par this book, This book does \'a40t C0l\lquote ld0l'le l'l\'a4F imply that Grill

Pl\'b0\'b0\'80\lquote The reasons Strike wrote this book. The reasons you\rquote re reading

\par dure listed herein be used by the reader or anyone else for that this book- Ecstasy is ins

most benign dmg Sinks has ever 9n_

\par matter. Even if the chemistry were legal Strike would not advise s\'b0umsi\'bbsd_ ii is

passive ysi powsi-iUi_ By pswsifui Siriks does noi

\par anyone to try these pr\lquote\'a4GedUl\lquote 9S U\'a4l9S$ ll`l9Y h6V\'80 3 th\'b0l\'b0U9h

U"' mean that it incapacitates or makes one dangerous. It is, in fact,

\par derstanding of chemistry, \'a4h6mi\'a4\'a4| F\'80\'a4\'a4U\'a4\'a4S Bild

m\'80thPd\'b0'\'b09Y\'b7 quite the opposite. Its power is in its ability to evoke a total sen-

\par Even the most basic chemical or reaction has the potential to do ssiy bath si issiiisi Visuai

and mental enhancement One.?) pen

\par great harm. - ception is perfectly clear. Halluclnations are nonexistent. The

\par feeling one has is, literally, ecstasy, Plus, it is one of the few nar-

\par cotics in the world that is not physically addictive. Why this sub-

\par stance was taken away from the people is a question that only

\par government-funded scientists can answer.

\par And let\lquote s not forget Meth (speed, crank, crystal). Then again...why

\par don't we just forget about them. Momma said if you can't say

\par anything nice...etc., etc.

\par Eml.Em.dlms

\par

\par G

\par < Bos ties

\par 0

\par MDA Anvhmmine

\par 3.4\emdash M\'a4Irvyl\'a4neDI\'a4\'a4yAmphet\'a4mlns (Blnzodrlns)

\par o cli, Hi

\par V 0

\par < (Def

\par MDMA Methamphetamine

\par :1,4-MelhylensEIuxyI|ethAmphatami1\'a4 (Spud)


5/246

\par


6/246

\par difference is required. Anyway, if one were to look at that nitrogen

\par atom stuck on the MDA or amphetamine core one can see that as (1) Little, local walk-up

type stores

\par more carbon groups are added on, the weaker the drug becomes. These kinds of stores carry

hobby/craft supplies, gimmicky sci-

\par So MDEA and PEA are even weaker than MDMA and speed, but ence fair projects, ant

farms and a low assortment of basic

\par they do retain some pretty fair activity. And a few pages away you scienceware products

such as beakers, thermometers, scales,

\par are going to actually learn every excruciating detail of how under- rubber stoppers and most

of the basic chemicals such as acids,

\par ground chemists make every single one of these compounds! bases and solvents. These

places are listed in the chemicals sec-

\par tion of any big city's yellow pages and are relatively safe places to

\par get most of the basic lab necessities. The drawback is that they

\par are really expensive and don't sell very large quantities of any

\par chemical. It is possible to have these places special order a

\par needed chemical as long as it's not a controlled chemical.

\par (2) Local middlemen companies

\par These places are also local businesses that can be found in the

\par chemicals section of any big city's yellow pages except that these

\par places have some big connections. By this Strike means that they

\par are licensed distributors for some of the biggest chemical and

\par scienceware companies and manufacturers. Those big compa-

\par nies would never sell a thing to a punk like you or Strike. Even if a

\par punk like you or Strike was to present a fake business front or

\par - g - \lquote 9 \lquote

\par

\par something they would scrutinize it very closely and would require

\par proofs of clientele etc., etc. What the chemist is looking for are product companies that sell

\par everything but glassware and chemicals. The reason for this is


7/246

\par lt's needless to say that this is too much to ask of a street punk. that if they know they don't

sell anything that is watched then they

\par That is where these distributors can help. They have the license have no reason to care who

buys their stuff. In fact, they want to

\par and authority to sell anything (both chemical and glassware) that sell the chemist stuff very

badly. The other types of catalogues to

\par the chemist needs and are not subject to the same policies that look for are those that accept

credit cards and. money orders as

\par lhs companies thsy sell fst smplpy- This is hst mssht as a put- payment. These companies

obviously sell to individuals. All or

\par dowrl but these dlStFlbUiOrS are like car S8|eSm\'80l\rquote l. The only way these

Companies are excellent places to stock up on everything

\par they msks mehey is lhi0\'a49h ths eemmlseleh eh sales- This the chemist needs, especially

low priced magnetic stirplates, vac-

\par means that they tend not to care about whom they sell these other uum pumps, plasticware

(great alternatives to some glassware),

\par cmp\'a4\'a4iss' products to- Thsy lust wsht ts ssll stuff- A chemist electronic scales arid,

in some instances, chemicals and glass-

\par Calls \'b0l'le sf llleee \'b0ol""Pe"lee and srdsrs $\'b0melhln9 elmple like e ware. These

companies areiust like local distributors only bigger.

\par thermometer or water and then pays for it promptly. Having then

\par established an account (a foot in the door) the chemist will have (4) Big name science

houses and chemical manufacturers

\par Qellled lhel e\'b0m\'a4e"Y'e lluel ih kll\'b0Wll'l9 lhel She (lhe ehemlel) is e These include

such names as Fisher, Baxter, VWR, Cole-Parmer,

\par g\'a4\'a4


8/246

\par to ust lllel speslelly shemlsel or Piece sf Qleeewele Tllele srs the big name science houses

and glassware manufacturers. This

\par thousands of such places around the nation, Canada and Mexico. is haoausa ll Wlll help to

havs tha sompar,y\'b7s aotual produol oata-

\par logue number whether one is ordering from a distributor or from

\par (3) National dlsttibulets the company itself (looks professional, bubbal). These really big

\par lf S Chemist were tv 90 clown to hsr i0\'a48i Ui`ilVel\rquote Slly 0i Qiedueie catalogues

are down at the university or the chemist can request

\par research school she could find science company catalogues in the prra from lhs oomparly

ltselh They also make exoeiient reference

\par library and in the divisional labs and offices of the research center. books ar-ld are just plalh

lrltsrastlhg to read and daydream ot the

\par Representatives of every conceivable scienceware company and day when one carl ardar

sush_ahd_sush an apparatus as is da-

\par manufacturer like to drop off tons of their catalogues in the hope plsrad oh page Whalovar

\par that someone will order some of their products. lf the library has

\par \'a4\'b0l'le\'b7 lheh llle ollemlel goes up ts one of the labs ello eeks So with catalogue or list

of items needed in hand it is time for the

\par Someone ll Sho could lako o look ol some of lhell catalogues- chemist to order. The

following is an example of how a typical call

\par This iis not a problem because the labs are full of graduate stu- Wlll proceed aud how tt

Wlll be hal-ldled by a ohemist no matter

\par dents Who are dying for attention. Some have so many cata\emdash what business sha

calls;

\par |QgU\'80?* they don't use that, if asked, they would probably give the

\par chem lst S0m\'80. __Rlr\'b7lglRlrlgl--

\par - 10 - _ ll -

\par

\par Customer rep: "Good morning, Blah Blah lnc." At times it may seem that Strike is implying

that buying from these

\par Evil chemist: "Uh, yes, this is Fake Name calling for Fake Com- companies is a cat-

and\'b7mouse affair that leaves suspicions high

\par pany Name and l need to order some items or possibly open an and traces put on one\lquote

s phone line. This cannot be further from

\par account." the truth. These companies want to sell their products. lf they had


9/246

\par Rep: "Does your company currently have an existing account with to file notice to the DEA

or demand documentation every time

\par us'?" someone called then they would be broke in a week. This does

\par not mean that a chemist should be careless. lt's just that if a

\par [They always ask this whether or not they werejust told that a chemist is Polltsi friendly and

Sman than almost anything can be

\par customer is a new one] had. And since, as this book will point out, most everything the

\par chemist needs will be unwatched, there will not be a great deal of

\par Evil: "No, we used to have an account with Rival Scientific Com- suspicion no matter what

the chemist orders. Just remember one

\par pany but they cou|dn't seem to get our orders on time." thing: the chemist never orders

anything to the same place she

\par Rep; "And what is your company's name and address'?\ldblquote cooks at.

\par [They ask this tirst because they want to bag the chemist as cus- Science dealerships aren't

the only places to get the stuff one

\par tomer or at least get them on a mailing list so that they can hound needs. At those mega

hardware stores one can find pure acetone,

\par the chemist later to buy more of their stuff] methanol, ethanol, toluene, methyl ethyl ketone,

DCM(as a con-

\par stituent of some stripping agents), sodium hydroxide inthe form of

\par Evil: "Fake Company Name, at Address OfA Friend's House." lye, and some acids such as

sulfuric and hydrochloric. These

\par precious tools can be bought there cheaply and in great quantity.

\par [ Delivery to an apartment address is unwise and there are very

\par few companies that will deliver science products to a P.O. box] Then there are other places

such as chemical waste exchanges,

\par pool supply companies, electroplating companies, photography

\par Rep: "O.K. Mr. Fake Name, what can we do for you today?" supply shops, agriculture

companies, specialty gas canister com-

\par panies and just about any place where a chemical can be sold.

\par Now the chemist rattles off the catalogue numbers of the things

\par she wants and the quantity of each. After the order is confirmed Finally, if one simply

cannot find the thing one needs then it\lquote s time


10/246

\par the chemist asks that the entire order be shipped by overnight ex- to hit the bibles of

industrial and commercial sources; "Chemical

\par press and has this added to the total bill. The chemist then asks Buyers Weekly",

"Chemsource U.S.A." and the massive "Thomas

\par for the purchase order number of the purchase she just made so Register". These three

source books can be found at most librar-

\par that she can include this on the payment she's going to send. The ies and contain the listings

and services of just about every busi-

\par chemist uses a reputable money order and sends this money or- ness in the country. No

matter what the chemist needs, it can be

\par der to the company via priority overnight mail. All this rushing ac- found in these books.

Even if it takes going one-by-one through

\par complishes two things: it shows that the chemist's company is a the listings, Strike can

assure you that the chemist will find what

\par professional, goal- oriented company, and it also gives no one any she needs and someone

that will sell it to her.

\par time to second guess a thing or establish a stakeout of the deliv-

\par ery site. The one source Strike does not condone is theft. If you steal then

\par you are a weasel and a coward.

\par - 12 \emdash - 13 -

\par

\par Now, one is going to see most of the older chemical reci es call-

\par WHAT TO BUY ing for all reactions, solvents, acids and bases to be held lin Pyrex

\par (borosilicate) type glassware because anything else will melt or

\par degrade when exposed to

\par all these harsh chemicals \'bb

\par GI-ASSWARE and conditions. This is no ( .

\par longer true! Any reaction, i ,

\par Ideally, the chemist wants a distillation kit with joints that are of the add')'\'b0" \'b0' m'X""9

in this it

\par size 24/40(don't ask). This is the most versatile joint size for ac- b\'b0Pk (Wat does _"'Ot

Ve' _.

\par commodating both large and small flasks. Speaking of flasks, the qulre dl"?\'b0t haatlng canin; *


11/246

\par type one wants these days are flat bottomed flasks, not round be dame '\ldblquote 3 p\'b0|

YF"\'b0F\rquote Y|' '

\par bottomed flasks. Flat-bottomed flasks allow one to heat on flat are (PP) \'b0_"

F\rquote\'b0'YethY'S'j\lquote\'b0` \'b7

\par surfaces such as a heating stir plate. In the first of many beautiful, (PE) \'b0\'b0\ldblquote

ta"\ldblquote\'b0"'\'b7 -I-ms '$ rj 5E\{O$\'a3;i\'b7RY

\par hand-drawn sketches that will appear throughout this fine book regardless \'b0f the Chem"

kssevxoki L

\par one can see the components and proper configuration of a regular cms

"\ldblquote\rquote\'b0)Ved\'b7 P\'b0|Yp"\'b0' FVNNE-'-

\par distillation set up in Hgure 1. Other pieces of glassware that are Wlene (PP) and

\par highly desirable but can be lived without or made (as shown later)

p\'b0'Ve)hY'\'80'\rdblquote\'80 (PE) _ are _ * l

\par are shown in figure 2. very inert and chemically

\par resistant to almost any-

\par \'bb\'a4\'b7;m\'a4m\'a4\'a4ia\\ thing this book describes.

\par NEMOMETER I \'b7 Buckets, tubs, funnels,

\par warren and all sorts of containers :\'b7,\emdash m=.ck

\par \\ of this whitish, opaque, "\}\ldblquote\ldblquote

\par ms in 3-,,,,, pliable plastic can be [Figure 2]

\par "\lquote 3`IE'\\ *5 Amvert found for pennies at any discount or grocery store. These con-

\par \'bb.&\'b0-ii\'e9k \'b7t\'a7i.= I 'I tainers are stackable, easy to clean, never break and will

save a

\par I \\_ chemist a fortune in glassware. As was mentioned earlier, plastic

\par VACUUM ER ` ware is starting to make its mark in biological and chemical labs.

\par _, Asker-sa coseete Buchner funnels, side arm flasks, graduated cylinders and even

\par separatory funnels come in PP and PE. These glassware substi-

\par N Immun X tutes are the absolute choice for today's chemists as they are un-

\par rmsk watched, versatile and 1/10 the cost of glass. lf the chemist is

\par \lquote unsure what plastic a container is then she can look for the letters

\par g PP or PE somewhere on the product.

\par surtvciwe


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\par . VACUUM

\par #~ec=1;v.t.NG

\par Fl.P\\5Y\\ \'b7

\par The chemist is going to need a source of vacuum. When distilling

\par [Fl9UV\'80 ll high boiling stuff like valuable ecstasy free base oil, a vacuum is

\par _ 14 _ - 15 -

\par

\par applied at the nipple (tee heel) of the vacuum adaptor so that the

\par pressure inside the entire distillation apparatus is reduced well HEATING AND S-I-

IRRING

\par below the normal atmospheric pressure outside. This causes eve-

\par rything to boil at a much lower temperature. If high boiling oils are . . _ _ _

\par allowed to dlstlll/boil at their normal temperatures and atmospheric Tl\lquote a"a 'aallll

'?\rquote "\'b0 g\'b0\'b0\'b0l S\ldblquote l?Sl'l\ldblquote\lquote a f\'b0' 3 \'b0\'b0"\lquote

b'""*'\'b0" \ldblquote\'b0*\rquote **"9 and

\par pressing than a considerable amount Of product could be lost dug magnetic stlmng plate.

nor IS there any reasonable excuse not to

\par to scorching. The other purpose for a vacuum is for vacuum filtra- ga? ana Tlgffjalabparlaclly lagal la buy and aan be mma at a"Y

\par tion which is a very useful process and is described later on. salanaa Ou a Ol a alll 200400

a\'b0llar$\lquote lalalas \'b0"a araa that tha

\par \rquote chemist should not sklmp on. Thls piece IS going to be the center

\par . . . . fevery action in the laboratory so a really good one with as lar e

\par Any commercially avaliable vacuum pump IS perfectly fine for the \'b0 . . . . 9

\par underground chemist\rquote s needs; but the best kind to buy is a dia- a sullaaa araa aspasslbla ls a daflnlla plus

\par ` ` ` t t th -h h h ' I . .

\par 52;%?;\ldblquote rE\'a7.'2ie\ldblquote ;Efl\lquote .Li.?.\lquote ;iZ*gl?iisr23;.$a.

$u$L\lquote i,'L...i'\'a7 .\'a7J;T.'\'a7S. ers was

S~\'a4\'a4\'a4se\'b7.\'b7~y\'a4\'a4the\'b7\'a4\'a4\'b7\'b7yr that the ~r\'b7\'a4er\'a4r\'a4~\'a4\'a4

creme is

\par $1OO_$2OO_ However the stronger the Vacuum the better. If 3 too stupld or unwllllng to

get a stir plate. In this case a single unit


13/246

\par chemist is looking to pun 1mm of Hg (dom ask) like tha gms in the portableihotplate can

work, but controlled heat using these is best

\par chemistry papers do than Sha can be looking at a turbovac that accomplished by water or

oll baths. Stlrnng can be accomplished

\par can run WSH Over $5000 by attaching a shaft and paddle to a power drill or any gear

driven

\par ' motor.

\par The other vacuum option is a simple little aspirator that attaches to

\par ones faucet or hose. This $15 device pulls a decent vacuum;

\par however, it is not an option at all in Strike's book. Running one of

\par these babies 10-12 hrs a day is a despicable waste of a commu-

\par nity\lquote s water supply.

\par WATER PUMP

\par This is going to supply the cold water that courses through the

\par condenser whether that condenser is set up for reflux or is part of

\par a distillation configuration. The pump need not be very strong. In

\par fact, the perfect example is one of those little, submergible fish

\par tank pumps that one can find at any pet store for about $10. All

\par the chemist does is attach a hose to the outlet, chunks the little

\par pump into a bucket of ice water, attaches the hose to the con-

\par denser and there it is. An alternative source is that little pump

\par that's attached to the windshield washing fluid reservoir of any car

\par in a junk yard. The chemist removes the reservoir (pump still at-

\par tached). applies an adapted power source to the pump and uses

\par the plastic reservoir to hold the ice water.

\par - 16 - _ U _

\par

\par HOW T0 MAKE The best replacement for borosilicate glassware is stainless steel.

\par Stainless steel takes the heat, won't break, and, most importantly,

\par is about as resistant to chemical degradation as the chemist can

\par _ _ I hope to find. For those items that won't be subjected to direct


14/246

\par Strike is Sure that an lmeglhetlve Pel\rdblquote S\'a4h Feh t\'a4\'a4k \'a4F\'a4U\'a4d her

eVe\'b7 heat there can be some steel/metal or steel/plastic hybrids. ln fig-

\par ryclay surroundings and think \'a4f S\'a4m\'a4tt\'a4\'a4\'a49 that can ast as 8 re- ure 3 is

shown now riasks or any size can be made with two

\par placement fOr S\'a4fn\'80 of th\'a4Se hefd to get 9te5SWel'e lteme and stainless steel

mixing bowls welded together. Also shown is the

\par other 9tZm0S\'b7 As it S0 hePPeh$ Strike hee th0\'a49ht eh_\'a4\'a4t this t\'b0\'b0- vacuum

adaptor and condenser. For the condenser only the inner

\par Here are S\'a4me 0f the m0Fe likely We!/5 thet theee thlhQe Geh bs pipe need be steel. The

outside pipe can be copper or something.

\par made. As for the other components of a distillation set up, well, they are

\par made just as they look.

\par EJ

\par 6 A_;_, In figure 4 is shown how a separatory funnel and a pressure

\par equalized addition funnel are made. The funnel part is just a PP

\par funnel from the grocery store and what it is attached to is a stain-

\par - ` ` r less steel ball valve. See how the addition funnel is made by us-

\par \lquote\'b7 ing a rubber stopper and an extra extension of tubing to the top of

\par \'b7 the funnel? Well, that's how one can make a sealed addition fun-

\par nel out of the ordinary glass separatory funnel that one gets with a

\par distillation kit or from wherever.

\par , I , J MQ I `\\ "

\par , 1 . ` J: _

\par @2% la" Sb- \lquote \rquote .

\par Q \rquote E \lquote "*\'b7~__\\ .

\par Z \rdblquote F)g;\'e9_M ' "*-...,_, . /

\par 13 Q3) . \'b7;

\par gf? JZ? _

\par U I /,2// // / f . _ _

\par r//\rdblquote 2* i ~ JY /\lquote r W r \'b72l\'b7~

\par 5/ )- \'b0 / at a . T


15/246

\par @t \emdash , in ~

\par [Fig 3] [Fig 4]

\par _ 18 _ - 19 -

\par

\par All of the pieces pictured here are not going to fit perfectly into

\par each other and that's going to cause all sorts of leaks. The an- \'b7 .

\par swer is teflon tape. Strike loves teflon tape! This inexpensive

\par product is found in the plumbing department of any hardware ,

\par store and is the duct tape of the next century. Teflon tape is \lquote `\ldblquote ` l

\par chemically and themially indestructible. This stuff is wrapped XQK " T`*"\rquote\'a4'\'b7\'b7~

\par around any piece of pipe or joint, said part then jammed into its xg; 1-/r=\'b7\\ hV_,rPr. _

\par appropriate receptacle and the tape will mold to form a perfect fit. _ 4 \'bb

\par Hell, it can mummify a whole joint complex to make it absolutely giQ ? *

\par impregnable. _ * "

\par i \'b7\'b7 tf?

\par So what's the downside of using a stainless steel distillation kit? ; \emdash

\par The chemist can't see shit! There is a dehnite advantage of being

\par able to see a reaction as it takes place and to see when some- -

\par thing starts to distill over. All Strike can say is that the chemist

\par must rely much more heavily on the readings of her thermometer

\par and have a greater faith in the chemistry she is doing. By this _;\rquote Z_

\par Strike means that since there is probably going to be no more ` gg?

\par than 2-3 different chemicals in the reaction flask, then all the

\par chemist need be aware of is what thing comes over first , second _ _

\par and last. Strike knows. Strike knows. lt\lquote s a little more complex `

\par than that. But if a chemist gets the hang of distillation it really can

\par be as simple as that.

\par [Fig5]

\par PIPE BOMBS


16/246

\par A pipe bomb is not a bomb, It is just a device to hold high boiling

\par or high-pressure reactions in an enclosed cell. The bomb should be GIRLS IN DA HOOD

\par made from a stainless steel pipe that has as big of an inner diame- Some Of the reactions

that the chemist ma _ .

\par . . . y use will ust naturally

\par mr F15 possible (w1dFh\rquote bubba!) Them argtwo good conngumtmns smell bad.

Usually if something smells bad then it\rquote s probably bad

\par wh\lquote\'b0i\lquote can be scm m Hgum 5* One em? ls permammiy sqalcd by for the

chemist to smell it. Some reactions are, by design, sup-

\par Wcldmg Thc \'b0th\ldblquote\lquote "\ldblquote d\'a4 H0 matter

Wh\lquote\'b0h_\'b0\'b0\ldblquote Hg\lquote\'b7\lquote\ldblquote\lquote\ldblquote P\ldblquote

ls \ldblquote S\'b0d\'b7 posed to vent bad things that , when unchanneled, have nowhere

\par Should haw as much end as HUG it threading as POSSlbl\'80\'b7 Also, to go but into the

living room of the chemist. Sometimes there is

\par when sealing up the pipe bomb, it is e great \'a4d\'a4\'a4 rb wrap at lor of he guarantee that

a method Will go as piarmeti. There may be a

\par teflon tape around the threads then screw on the cap. This will mistake or unforseen side

reaction and some of the most deadly

\par form an absolutely air tight seal. It is also possible to substitute a shit imaginable can be

evolved. That is why the chemist will con-

\par stainless steel pressure cooker for some sealed, pressured reactions. Struct

lh\'80 \'a4l\rquote l\'80 thing that may Bhd UD 59Vlh9 her life: 3 fume h\'b0\'b0d\'b7

\par _ 20 _ \'b7 2l -

\par

\par ln professional laboratories fume hoods are big metal boxes rest-

\par ing on countertops and are connected by ducts to blower motors A fume hood is constructed

in the manner shown in figure 6

\par on the roof of the facility. The blower motor is constantly sucking Strike drew the frame as

being made of lumber but it can be made

\par the air from the hoods to the outside so that chemists will not be of rebar or, preferably,

from PVC pipes and joints so that it can be

\par exposed to the vapors of chemicals they are working with inside assembled and

disassembled with ease. The frame is enclosed

\par the hood. The same precautions are taken by non-dead under- with plastic drop cloths or

any semiolear plastic sheeting. The

\par ground chemists. front face of the hood is halfway covered with plastic while the


17/246

\par bottom Vhalf is exposed to allow one to move objects in or out and

\par to rganizulate things. On top of the chamber is attached some

\par , -\lquote \} cot es ryer duct or some such crap which is led to a leaf blower

\par my \lquote __r VV VV .... or blower motor. The exhaust from the blower is led away tothe

\par . \emdash a \rquote \ldblquote :\emdash\'bb\'bb \'a4\'a4*Si\'a4=~=-

\par V .\'bbT_`;VV y . .;V.W W .V Although a leaf blower is probably way too strong it may

still be

\par \emdash _V V = adequate at its lowest settings To insure that a correotairilow is

\par . V V V . V T QV., gleing pujled the chemist; holdks 1 lit cigarVett: about a foot

in front of

\par 1 Mx i \emdash - v VL Zi_q, Q V,\'b7\{ .5;;% e oo s opening an oo s o see i t e smoke

trail is being

\par VV I .\'a4 _j -~\'bbt pulled into the hood. lf so, then the hood worksjust fine.

\par V Many houses have outside\emdash venting blowers over their stoves.

\par \'b7 ~ Chemists in these situations can actually drape some plastic

\par "~\'a2~ V \'bb\emdash ., V6, around their stovetop to make a perfectly adequate hood.

How-

\par ; ever, chemists who live in apartments never, ever attempt any

\par _,Qt. . \lquote \lquote ff chemistry at all in their pads. Why'? Well, not only do

apartment

\par --\'bbi Qi- stoves lack an outside vent; but to vent a constructed hood

\par _,,. g V V fi V through a chimney or out a window with so many close neighbors

\par [ . . V \lquote \'b7\'b7\'b7\'b7 Vi_f \\_;.._ _ ;\rquote is ~._V \emdash > living about

is just plain stupid. lt is also stupid in another very

\par \'b0 \rquote \'bb Q important way. If a chemist fucks up and blows herself up or

\par \lquote V V starts a fire then she is not only harming herself but is also going

\par . . V to put a lot of her neighbors out on the street, in the hospital Or in

\par the morgue. No one making drugs has the right to jeopardize oth~

\par _ ey O ers in this manner. That is why drug making is always done in a

\par I house, barn, mobile home (watch out for tornados), submarine or

\par .\'b7.... *2 cave.


18/246

\par [Fig 6]

\par - 22 - _ 23 -

\par

\par M ETH0d0I0gy

\par lf the chemist has done the appropriate thing and bought a heat-

\par ing stirplate then a magnetic stir bar is always stirring in the reac-

\par tion flask. lf the chemist only has a hotplate then the chemist is

\par Just in case you are not familiar with basic laboratory procedures, Qeing to have to add

Some boiling Stones to the flask. Boiling

\par this chapter will explain them to you. These are the most basic lab stehes Gah be either

little Chips of teflon. little wedded up balls of

\par techniques and almost every method in this entire book will re- teflefl tape Of little pieces

of a shattered porcelain countertop tile,

\par quire many, if not all, of the protocols to follow. So pay attention! All ef these things have

lets of ltliefescbpie p0Cl


19/246

\par There are three basic forms of distillation: simple, vacuum and Ptedueti all that pure

Sell/ent that Comes over first is perfectly re-

\par fractional distillation, which oan toe an extension ofthe first two. usable and elleuld be

saved fer future exlraetlens.

\par Simple distillation is just plain old distillation with no vacuum and is

\par used for purification of low boiling mixes or for removing solvents The laet thlh9 about

dietillatieh that heeele lhel'ltiellil'l9 is the sWsP\'b7

\par such as ether. For vacuum distillation a thick walled or reinforced nine eut et eelleetlen

flasks When distilling under vacuum it will

\par hose is connected from a Vaouum pump to the hippie (too hooi) or be necessary to remove

the flask that has collected all the solvent

\par tha Vacuum adapfgn Application of a Vacuum graatiy reduces tho or crap and replace it

with a clean one to collect all the product

\par temperature or boiling and is a must tor most ofthe distillation in that Will be Pelnlns ever

elleltlv- This swapping ef flasks needs le

\par ~this book. Fractional distillation is merely vacuum distillation ex- bearlene \'80luleklY as

seen as the Veeuum hese is diseehlleeted- By

\par cept an addod oiaoswara oon-ipononr such as a Smaii Vigreux ooi_ quick Strike does- not

mean lightning fast. Just quick enough so

\par umn or a Ciaiaon adaptor packed with shards of giaoo is piaood that the hot solution in thereaction flask does not get too much

\par between the reaction flask and the 3-way joint of a normal setup. hettet hem llie heat seuree

it is elttihg ehi because it it dees. ehd

\par Either of these additions create a gauntlet of extra surface area the Vacuum le leaphllet-l- it

meV pull e little tellh etthel suPel\rdblquote heet\lquote

\par elements that distilling liquids must pass through in order to con- ih9 etuht and Qe elsleeshl

inte the eehdehseh

\par dense. This affords a greater degree of separation between

\par mixes of oils that have similar boiling points. However, it has been REFl-UXlNG

\par Strike's observation that most of the bulk separation in this book

\par using distillation ean be achieved with regular old vacuum distilla- Refluxlno ls all ever lllls

beek and the proper annaralus le use is

\par tion. pictured in figure 7a. The most general thing that can be said

\par \lquote 24 \lquote - 25 -

\par


20/246

\par _ _ __ _ concern when refluxing large aqueous solutions such as acid or

\par about refluxing is that it's lust plain old boiling except that there is bass nydrslysls seen lalsr

lrl lhls book

\par a condenser attached to the flask so that nothing escapes. The

\par condenser must be supplied with really cold water, especially

\par when refluxing hi9h b0iiihQ Sdiuiidhs- One side note about the drying attachment is that it

need not be a

\par vacuum adapter. Anything, such as a funnel, that can hold a plug

\par ro., of drying material and tit snugly into the condenser will work.

\par 2

\par I? EXTRACTION

\par V A \'b7 In this book extraction is almost always about using an organic

\par solvent such as benzene, DCM, ethyl ether (a.k.a. ether) and hex-

\par , *\'b7"?iS\'a5\} ane to remove (extract) product (almost always in oil form) from

\par .l-n an aqueous solution. The most basic way to extract is to pour the

\par .. ` water solution into a PP container, add some solvent and stir the

\par . two as fast as possible for a few minutes. Most equipped labs use

\par ,- a large separatory funnel to shake the two liquids. When using a

\par separatory funnel it is very important to vent the funnel as soon as

\par the stopper is smacked into the top. This is done by immediately

\par V or _.=. _ inverting the funnel so that the stopcock end is facing upward,

\par opening the stopcock to release the pressure then closing the

\par . stopcock. The sep funnel ls given a quick shake then vented

\par @ again. This is repeated a couple more times after which the pres\emdash

\par . sure production will have pretty much ceased. The rule is to then

\par [FiQ 73] [Fig 7b] shake for 2 minutes and allow the layers to separate for 10 min-

\par utes. And which layer is going to which? Ether and benzene are

\par always on top of water and DCM and hexane are always on the

\par You see that vacuum adapter stuck to the top ofthe condenser in oollom_

\par fig. 7a? Well, a closer look at it in fig. 7b will show that it has


21/246

\par Some drying agent sandwiched between iW\'b0 \'b0\'b0ii\'b0h haiis ahd ihe Most science

papers call for things to be extracted 3 times (3X)

\par nlppl\'e9 USG hed!) $98iBd With Piasiic Wrap O" f\'b0ii- The dU/ing ag\'e9ni with a

solvent. Strike feels that this is overkill and that one or two

\par can be either a commercial product called Drierite or calcium chlo- llmes is usually

eufflolenf Sometimes one nas eo much product

\par ride. This attachment is Didded on i0P of \'a4 condense" Wh?i`* i\'b0\lquote oil that it

forms its own heavy layer (usually at the bottom). There

\par fluxing solutions that have no water in them and must remain that ls no need to exlraol

Such a large amount Wlln eollrenf ln Such a

\par way during the time they are refluxed. All this is to prevent m0is\emdash Case one would

merely draln lne oll from me wafer on if using a

\par ture in the outside air from coming into contact with the cold sur- pp container, deeanl the

wafer from me oll_ The wafer llseif can

\par face of the of ih\'e9 inside walls Oi the C\'b0nd\'80h$9i\'b7 This will $ui\'80iY then be

extracted once with solvent and the solvent added to the

\par happen and the condensed outside-air water will drip down into oll_

\par the reaction flask and ruin the experiment. This is not so much a

\par - 27 -

\par -26-

\par

\par WASHING .

\par ter free, bubbal) for some of the recipes in this book that call for

\par Washing is almost always the act of taking an organic solvent auch IIIIIIgs\'b7

\par layer (most likely the one that was obtained from the extraction of _ _ l _ _ _

\par some previous aqueous solution) which usually contains product FIW'"9 '$"'I ?bS\'b0IuI\'b0IY \ldblquote\'b0CeSS?W\'b7 but ll 'S 8 9\'b0\'b0d Pet Illat tf 3 l'\'80\'a2\'b7

\par and mixing (Washing) Clean Water than discarding the Ip\'e9 SITGSSES ItS USB

th\'80l`| Sh 6Vll Und\'80l`gTOUl"ld Ch\'80mlSl will do SO.

\par water. A solvent layer is often washed with a dilute acid or base

\par salt solution to neutralize anything the solvent may have absorbed VACUUM

FILTRATION

\par from previous extractions. These salt solution washings are then _|_h_ a _ a t l t "_ a a f

\par followed by clean water washings. IS proce ure is use o separa e crys a ize pro uct rom sol-


22/246

\par vent or to remove crap and solids from a liquid. Figure 8 shows

\par Since we\lquote re on the subject of clean water, this is as good a time as the tamper

appafalus to USG. The ciollecting flask is called a side

\par any to discuss what kind or water is used in ati this chemistry. By arm ask aud to

that_e>


23/246

\par a shot glass full of sodium sulfate (Na2SO4) or magnesium sulfate .5 23:2 \'b0 S B Ig afclh

IIa\'b0S IIIG \'b0k.\'b0IIIIS Iy a

\par ls dumped into the filter and the solvent poured through it. It is Ish lhV\'b0I\'a5l \'b0II. ;I

lleh IIIg`IIIa \{Il? pflmiss ..\lquote `

\par also a good idea to follow up by rinsing the Na2SO4 with a little gag? af .GlmIS fYIII l

avekczyif $9 GC; .

\par extra, clean solvent to insure that everything gets washed out of lh as SI ln \'b0 a matt TSI 6

a B t\'b0[mllaII

\par the drying agent. The NHZSOA is a white crystalline salt that tastes lh\'b0" 'l\'b0\'b0 flh\'b0

s\'b0F\rquote ?'a P \'b0s\'b0 WS a S '\'b0'\ldblquote F. 8

\par like table salt. It binds water molecules without readily dissolving 6 S\'b0 Ven GY me III I

Ig I

\par and leaves the solvent water free. This way of drying is also an

\par option for making some solvents and pure liquids anhydrous (wa-

\par - gg -

\par -29-

\par

\par PRECURSORS thing easier for all involved the chemist informs the company of

\par the fake name of her business and that she makes soaps, in-

\par cense, potpourri or is an aromatherapist (no kidding). Other

\par places to order essential oils would be home care products

\par SAFROLE houses, toiletry base companies, soap companies, flavoring com-

\par panies, aromatherapy stores and organic foodstuff companies.

\par Where te eeehh Where t\'b0 baglljl Wa"- $*;**09 Vlftlintlgs Ghaptal is As of the year 1998.

small quantities of sassafras oil are still being

\par a 9\'b0\'b0d 'dea\'b7 Every awphetahhhe IS a e Emleg 2 elheelyglir sold on retail shelves

without any scrutiny. Usually in 1-4oz sizes.

\par geyerhmeht deeegt a ew lehe tgqewh eil ry . e el em ea 'le \rquote Anything larger is

usually sold only through distributors and

\par \'b0he has te. ge a eet hha 'hg e amp eahhheh rehh lega (er manufacturers. And as of 1998,

the DEA has informed most of

\par $\'b0ma*"\ldblquote aa "'agah \'b0*\lquote a'\ldblquote '\'b0a'a that alias F\'b0laa *\'b0l a

lm? lhgeaa these distributors that they (tits DEA) want lists kspt or saiss rs-


24/246

\par p\'b0Sa'e'e\'b7 Fer e\'b0ataSy\'b7 that etarhhg e ehhea 'S a mee aways a` ported of most, if

not all, sassafras oil purchases. Mind you it is

\par hole not illegal to buy the oil. lt\rquote s just that you will be put on a list if you

\par .Th t\lquote " dSbt \rquote . lt\lquote :

\par Safrole is the #1 starting material for making X today. As a pure ggve

sgmceasjleaeygetgcryllegci\'e9i Watche U S ance S0 U me

\par chemical it is a schedule l controlled substance and, obviously, is '

\par mega! te ewh er buy yhtheut a pemht /\\O Strike has also been poking around the DEA and

is getting the

\par But, safrole IS. th? m\'a4l\'a4F \'b0\'b0ml$\'b0lqeht tel distinct impression that they will

very soon reschedule sassafras

\par the eeeeheal ee e essafias W Ie. Ie S I O oil as schedule I. Then one won\rquote t be able toget it at all without a

\par quite legal to obtain. Sassafras oil has a pennll el Some Serleus decepllen

\par strong licorice smell which is imparted to `

\par lt. eem the eaeele melecele Cemhlgee \\ All of the above safrole/sassafras oil sources are the

more stan-

\par elahyx there are \{we klhee ef eaeea ras . - dard avenues to get these commodities. There

are some rather

\par oil being sold today: American sassafras (Sassafras albidum) and exelle Sources Of safrole

for the desperate gel/elnmen_

\par Brazlhae eaeeaeae (oeetea eymearem) Plam. ele Ameeeah See` tally-challenged citizens of

the future. Certain kinds of Asian cam-

\par safras contains about 80% safrole but the Brazilian sassafras oil is nner Olls esneclelly

blown campncl ell cen eenleln 4060%

\par ahheet ee`ee% eahele and eah pretty mech ee eeee as le safrole (another term to look for

is \lquote Camphor 1070'). Sources

\par . . ll` ' rt`f` ` l f `l' ll ll` ' f 50\lquote V

\par So where does one go to get sassafras oil'? Well, if one werelto Zgnngelni ellgzozeiiirgeg

eA;nl\'a7l:ec;\'a7t;?eae5;enlgeele;1\'a7i OApnle`;

\par go down to one of those sickening hippie health food stores or in- eleble amounts of safrole

can be found ln Slel enlse ell end

\par cense shops there, on the shelves, will be small bottles of 80-90% smaller amounts can

found ln the Olls Ol, elnnemen mace 'belel

\par ecstacy starting material labeled as sassafras oil. Larger quanti- leaf and nutmeg (lots Ol fun

lnlngs ln nutmeg)- Alec, lhelfe ls a


25/246

\par hee areereeree rather eheshly "\'b0'\ldblquote .*a:\'a4'a"\'b0a er pahuma eeplely spice bush

that grows in India called Betel. Betel leaf oil can be

\par eerhpamee that ehe eah he lh ahy ele clv yehew pagee New e found commercially and can

contain up to 40% safrole depending

\par people at these companies aren't stupid. They have a general On lne leglnn llwes eulllveled

ln

\par idea of what some of their essential oils can be used for so they '

\par mlght ask. But they still have no legal reason notlto sell these The sassafras tree llsell glows

llke e Weed ln the Wllds and along

\par thmge te the ehemleh After a"\rquote the Sams Stuff le eemg Sele ever disturbed fence

lines throughout the south, southeast, eastern

\par the counter to hippies just down the street. Just to make every-

\par - 30 - - 31 -

\par

\par Qsual Components of Sassafras Oil

\par seaboard, and Appalachian mountain regions of the United

\par States. The trunk and root bark of older, mature sassafras trees Component range gf aaatam

baiih-,gpO1nt@1a1m(OC)

\par can be steam distilled to afford the safrole-containing oil. Another

\par source of safrole would have to the be leaf oil of a little shrub that pihaaa 2-1g% 154

\par grows down in the low woods and swamps throughout the coastal phaiiandrano 2-1g% 175

\par plains from Florida to Georgia. The oil is more than 90% safrole d-ggmphgr 5-5% 2g4

\par [61]. The plant is known as Illicium parviflorum michx and Strike Safroia 39-99% 234

\par has no idea what the hell it looks like. eugenol O-10% 252

\par A new source of safrole that Strike has just stumbled upon is in [Table 1]

\par Strikes back yard. Momma comes home from the local nursery

\par with two plants that have these enormous leaves. They are suc- No matter what the safrole

content is, even that of the Brazilian

\par culents and grow like crazy. Strlkei `\ldblquote Whal l/8 90l there lVl0\'a4\lquote lh\lquote

l\'a4?\rdblquote sassafras oil, it is always a good idea to try to get rid of as much of

\par Momma: "Don\rquote t think I haven't notioed those filthy drug books you the other

components as possible. The most basic way to do this

\par write, you sick little mohkeyl" Strikei \ldblquote AW 0\rquote m0fl. lVl\'a4m\'b7

Lel'S \'a4\'a4l is to throw all of the crude sassafras oil into a PP container and


26/246

\par get into this again. Strike doesn't...\rdblquote Momma: \ldblquote WeIl I needed stir it with

an aqua] amount or 3-5% sodium hydrgxjdg (NaOH)

\par some new ground cover plants, ahd...Si9h...l know l/Ol-l'l\rquote e ll'\'a4t0 this solution.

Little white crystals of eugenol anion will form in the we-

\par twisted licorice thing...so l bought these weeds that are called ter layer. The water layer is

poured off and saved. That eugenol

\par \lquote Licorice Plants\rquote ." is valuable, Eugenol is usually the main contaminant in

safrole in

\par more ways than one. lt is the only molecule in sassafras oil that

\par Strike breaks off a piece of the plant and smells it. Oh Yeah! will react the same way as

safrole so if it hangs around with the

\par That\rquote s the bomb! The plant is called Piper auritum. Its common safrole it will

compete with safrole in the conversion reactions.

\par name is Hojo Santa. Strike loves Strike's mother. Also, eugenol is about the closest to

safrole in both structure and

\par _ boiling point so that trying to get rid of it by fractional distillation will

\par Suffice to say that anything that remotely smells like sassafras oil be very tough indeed.

Anyway, after the eugenol/water is poured

\par or licorice or any of those strong rustic spices is going to have off the oil that remains is

stirred with 3 washings of clean water.

\par some amphetamine precursor, maybe not safrole exactly, but The cleaned oil will look a

little cloudy now. Strike still does not

\par detinitely something. There is just no other substitute in nature for know why. But it never

seems to hurt anything. After the third

\par the aroma these unique compounds give. washing is poured away from the oil, the oil is

transferred to an

\par ordinary cooking pot and boiled at 100\'b0C for a few minutes to boil

\par The sassafras oil that one gets these days is not only going to off all the water. What would

you think of french fries cooked in

\par have the safrole but is usually going to have some amount of each that oil, huh?

\par of the compounds seen in Table 1 [6].

\par Strike wrote the above paragraph relying on the few accounts of

\par sassafras oil content that Strike had at the time. Since then, Strike

\par has come across more substantial data showing that Brazilian

\par sassafras has NO eugenol in it. This agrees with the claims of


27/246

\par many bees who have stated that no appreciable recovery of

\par - 33 -

\par - 32 -

\par

\par eugenol is obsenred when washed with the dilute NaOH. Strike . _ _ _

\par has also had commercial samples of both sassafras and brown top 10 recmes mscussee ieier

The one p"\'b0b*em W***`* ****e **`*e***od

\par eamphor analyzed for components and the results showed that Is that havmg Peer d*Stur*?

ed\'b7 s\'b0me \'b0f the sa**'\'b0*e m\'b0*e\'b0u*ee'

\par there Wee no eugenol in either. SO give it e ehet with NaOH er double bonds will tend to

migrate or reform ln the more energeti-

\par eemv Smke nelenger feelememmetterei cally favorable position between the alpha and beta

carbons.

\par What was all that egghead shit Strike just said? Strike said that

\par The above procedure Wee e good Step tewerde purity and mev be not only will safrole

reform but there may also be a small amount

\par all that one can hope for without a distillation apparatus. For Of *S\'b0Saf*\'b0*6 that

f\'b0rms ee We"' A*_s\'b0i S\'b0me Very *n*Lt*t*Ve Bees

\par those that have a distillation kit its time to get rid ofthe rest ofthe have s\rdblquote99\'b0$*?\'b0* **is* '* Weil be Possible *0 o0\'a4\'a4e


28/246

\par lt will be a little tricky but one can also try to purify by freezing! nPunfical\lquote i0n of

Sassafras Oil v2.0

\par The sassafras oil is thrown into the freezer to chill. Safrole itself _

\par freezes at -14\'b0C so anything that starts to freeze prior to that can The Seeeefree

P*e\rdblquote * \rquote s ep e\{\lquote Ge/lent source of Safrole. .8 Ilighly

\par be cold filtered in a prechilled vacuum filtration setup. The filtrate useful \'b0o\rquote

*Ypou"d\'b7 The P*e\rquote **V\rquote e*d$ UP to e%_ olt bl! Ws\rquote 9h*i Wh/Ch is

\par goes back in the freezer until -14\'b0C is reached and the mother en eXeeio*t\rquote

o\rquote Ze\rdblquote\'bbV good Weld- Sessefres ls mdigsnous **0 Vifgililsi

\par Iode of safrole freezes up. This again is filtered cold but this time the Cerolme S\'b7

Tenneegeee end Pens of _Ca"*ede\'b7 The prefeqred

\par the frozen mass of safrole crystals are washed with some ice cold meiiiod of eX*\rquote

ee*"`*g o\rquote * o\rdblquote * of *`*`*e _P*o"* 's oY Steam Dls*l\rdblquote 6*l0'*\'b7

\par methanol or ethanol (preferably at -14\'b0C) to wash away the unfro- The most eomrnon

method of oo*e\rdblquote '*\rdblquote\rdblquote *Q Sassafras Oil, U'*0UQ*'*. is

\par zen high-boiling constituents. oV P*\rdblquote o*"ee"79 \rquote * J`\}-

\par lf one is absolutely serious about ultra pure safrole then it can be

egg;g$r;t(\rquote\rdblquote ;n;I,E,i/iss/Qtlal OHS by GUS,-Ith\'e9n Sasse-

\par separated from the eugenol-free sassafras oll by treatment with

\par mercuric acetate [1,2,3,4] which likes that terminal double bond 80% Safrole

\par that only safrole has. The Hg(AcO)2 latches on to safrole at that o \rdblquote

\par double bond bringing it into solution as a solid; sort of like the way 106 Phellandreng

\par that eugenol was. The safrole can then be separated from its still 7% Cemohor

\par oily buddies by vacuum filtration. Safrole is then regenerated to 3% Eugenol & various

Sesquiterpenes (Cadinene el al.)

\par its normal oily form by treatment with hydrochloric acid (HCI) _ _ _

\par which flicks the Hg(AcO)2 off the safrole and the safrole double I he"e derived e prooeoe

for P\rquote efe[e\rquote **'e\rdblquote V sePa"a*"'*Q **`*e Safrole

\par bond reforms. As it so happens, the mercuric acetate also re- ou* of Sessefres _O'*\'b7 This

Process is based OP ***6 Physical P"oP\'b7

\par forms intact so that it can be reused again such as in one of those erilee of me Venous

somPo\rquote 7e\rquote 7*`s listed above combined W'*h 8

\par /iff/e chemistry knowledge. The normal means of purifying Sassa-

\par - 34 -


29/246

\par - 35 -

\par

\par fras Oil is through packed column vacuum fractional distillation. double boiler setup

(especially since this will take quite a while

\par This is an expensive, messy, and difficult process - in short, im- depending on how much

you have to distill/evaporate).

\par practical. My process that l am proposing takes advantage of drf- _ _ _ _ _

\par ferential solubility among the various oils in acetic acid to separate 5) Aftsr

d'$t'//8t\rquote\'b0" t9\rdblquote [""atES (Ethanal bc"/S at 78-4C),_f6S? your

\par the mixture down to only two components. The two remaining oils ggfmle PS"'? ms

PhY$'\'b0a\rquote Pmpamas data be/cw tv COl'Wl'm purity.

\par have sufliciently different boiling points to make simpledistillation, \'b0\'b0'9t'\'b0a\rdblquote % Yourpmduct $,70**/d ba b\lquote

-\lquote\rdblquote\'b0" than 99% PWS HOW.

\par with or without vacuum, a feasible separation method. To wit: Sa- Th 1 f S r I \ 'b7 L . - - . .

_

\par frole and Phellandrene are left, Safrole boils at 232C while Phel- S Sn ry Or 8 m 9 In angss

mdlcatss the fo/lcwmg pmpgmes

\par landrene boils at 171C. The difference of 61C is large enough to

\par permit excellent separation of the two, though some texts feel that Safrole 3, 4-

methylenedioxyallylbenzene - Bielstein ref # XlX\emdash 39

\par there should be 8OC difference between distillants (see Vogel), it Molecular Wgight. 162

19

\par is generally accepted that fractional distillation is necessary only . . . _ l

\par when the boiling points approach 25C of each other (see Zubrick). Svacrfrc G\rquote

a"\rquote t\'b7V\'b7 1- 100@2OC

\par However; with information newly acquired you now dont even Melting Point: 11C

\par hlavzgoddoggesziztillation, since Safrole is soluble in ethanol, while Bojlfng point'.

233_234C

\par e n e r . _

\par p A lnsoluble rn waten Soluble in Ethanol, Miscible with Ether and

\par Enough of the arguments, let\rquote s take a look at what rs going on Chloroform

\par here. . _

\par _ Note that this procedure has been modiried from the earlier ver-


30/246

\par Materials \emdash -\'b7\emdash -- Separatory funnel (2x volume to contain) Simple sion in

that we no longer distill off the Phellandrene, rathen we

\par Distillatron setup or pot on stove ,\'b7-) _ target its insolubility in ethanol as a means to

separate it from sa-

\par . . . . . f . ' k \lquote \lquote

\par 1) First wash with a volume of Glacial Acetic Acid equal to the mls Uhm We can all agmg

that this IS a much betmr Wayr Sh?

\par amount of Sassafras Oil being processed. This will remove Euge-

\par nol, Pinene and Camphorfrom the oil. This procedure, Strike believes, was not tried by

Eleusis. But his

\par 2) Wash with water to remove any salts made from other contami- $:1;,% Q; 21;

afjrjfb\'b0aQ;jLS\'a7;.'*L*j;Q'*\{1(;S gigs \'b0'du agdl f\'b0\ldblquote\'a7\'b0\'a7d\'b7

\par nants and to crash out any partially dissolved Safrole (it might .1-DK. ymmracted 8

1,11111;) pine resggch ?abOraiO\'b0:yrtO\'80;V\'801 Hi;

\par emulsify from the shaking, if so, add common table salt to help it proposal Here is what

they said, ppy

\par crash). ` ' -

\par 3) Wash with rectihed spirits (azeotrope of Ethanol + waten also Posted by TDK On

December 28* 7997 at O1`.28\lquote -34:

\par known as "grain alcohol') to dissolve the Safrole, leaving the Sassafras Oil

separation/purilication

\par Phellandrene behind. Of course, one should use only the amount

\par of alcohol necessary to dissolve the expected yield of Safrole. 1:1 \'b7 - . . .

\par seems to work, but could be an excessive amount. Zgglgfnp and IS WSH Swtgd for

Someone Wuhout any

\par 4) Setup for simple distillation, on the water bath, or if you don't \'b7 . _ .

\par wish to recover the alcohol (shame on you) just heat gently with a Slamng Weight" 112grams Sassafras O"'

\par Placed 454 grams of 28% acetic acid in 2 liter separatory funnel.

\par - 36 - - 37 -

\par

\par _ recipe Strike knew of at the time. There are numerous basic refer-

\par Using 25% acetic acid allows the eugerw/, d-G\'e9imptwf Hfid Pili\'e9lw ences for it inthe

literature and a couple of very convincing exam-


31/246

\par to form its own top layer. There was no separation using 99.5% ples in tha landmark book

~p|HKAL\'b7\'b7 by Alaxandol, and Am

\par acetic acid, Shulgin. Pioneers in the research of amphetamines they are.

\par Added 112 grams sassafras oil. Shake for a couple of minutes. ggygasa ?;V\'b03dShi;;ugh

f\'b0r Strike SO S\'b0m\'b0\'b0"6 Other than Strike

\par You get an orangish emulsion. Clears within 15dminutes f;:>r+m;2g -

\par oil, to la er acetic acl , eu eno e _ _

\par gvggiaggxb/gguggpggigd me ,5, fri\'e9m the Others) waghgd ma ci; What happens when

isomerization is performed is that the double

\par iayer 2x with fresh dH2O. Weight alter acetic acid & water washesi i\'a4\{i\'a4if\'a4i the

aiiyibenzene safrole migrates to the more energat,-

\par 1g1_5 (-10_5 grams) Ga ill Hilurabi\'e9 p0Sltl\'a4n between the alpha and beta earbons crthe

\par _ propyl side chain. Thus isosafrole, a propenylbenzene, is born.

\par Added 100 grams denatured alcohol, no layer fomwed as the oily

\par product is miscible in ethanol. Added 20 grams of dH2O. This

\par puiied the ethanol and other product into the t0P /6VSH b0ii\'a4m To isomerize safrole to

isosafrole one would like to have pure ea-

\par layer ccntaining Same ethanol and safrole. Sepafat\'e9d IHYGFS. frole to start with. This,usually, is not the case. Quasi-pure safrole

\par placed the oily bottom layer into a 2-liter breaker Took the temp from sassafras oil is ok.

Straight-up sassafras oil is probably ok

\par right to 234 C. The ethanol and water came off


32/246

\par Beautiful. `i`DKi B9\'a4UiiiUi\'b7 Strike, Suspects we wm be Seeing mma has no water.

The closest one can get commercially to anhydrous

\par from this Qifi\'e9d Gii\'e9misi i\'a4i\'80V\'b0" in the b\'b0\'b0k- ethanol is Everclear which

is 95% ethanol and 5% water (190

\par proof). A lot of chemical supply stores will not carry 100% 200

\par i$O$AFROi-E proof) ethanol because it is a potable (drinkable) producto \{This

\par / _ means that they would have to get a liquor license or some other

\par At this point the Gh\'e9misi has what can be i\'b0\'b0$\'80iY 'wnsideied a? state permit to

sell the stuff and that is a hassle that many don't

\par pure safrole. She can use this for some methods or can convert it want to bother with

\par to isosafrole for others. Isosafrole is the runner-up precursor for

\par making X. lt cannot be found in nature but rather is made from al-

\par most exclusively safrole. The 95% ethanol of Everclear is not an arbitrary concentration

that

\par P O the producer decided to stop at, mind you. lf so happens that 95%

\par Strike had previously written that about O ethanol and 5% water is a constant boiling mix

that no more etha-

\par the best recipe for making isosafrole nol can be purified from. That 5% water is there to

stay! There are

\par was from boiling safrole with concen- ways to remove that water such as producing a

ternary azeotrope

\par trated KOH (Potassium Hydroxide) in / by the addition of benzene, but they are kind of a

hassle and may

\par ethanol. This was actually the only 39

\par -33-

\par

\par not be necessary. Why? Because an alternative reaction for iso- _

\par mcrlzallon would bc to use a salulalccl aqucous lwalcll Zak) KOH still be dark regardless

and washing this ethanol with water at this

\par sololloo locloacl of an alcoholic ooc_ Thls wlll lalso loc lcmocla_ point cannot be done

because water is infinitely soluble in ethanol

\par ture of reflux to over 200\'b0C but is not too bad an can be used if (and Vlsa versa) $0 Wl/0

la!/GFS will not form.

\par desired. So, if it is ok to isomerize in pure water, then the little bit


33/246

\par gicgil\'e9falggilhi@ll;SxE;$:;;;;ui;\'b0:L;Zt em thmgs t\'b0\'b0 greatly Filtered or not, the

ethanol/isosafrole/(sometimes junk) is relieved

\par \lquote of its ethanol by openly boiling it on the stove or by distillation. A

\par . . . _ FW

\par ethanol removed by distillation is saved because it is clean and

\par What are some of the alternatives for this procedure? Well, one

gzgjlgtlxgfugableo(rjl`nin\'a3l?\'80r\rquote il will stl\}? have that 5% Water\} One

\par can use NaOH (lye) ih place or KOH out the yields will so down. ol all

ll'l'\ldblquote\'b0`l\'b0f \'b0 E S0 Venti ls Wall b'=\lquote\'a4\'a49S\'80 things can

\par Also, what about using denatured alcohol instead of pure ethanol? Q rc y \'b0 rea Y ast ast 6

last \'b0f the ethanol b\'b0"S awa!/\'b7

\par Denatured alcohol is ethanol contaminated with 5-10% methanol.

\par The methanol is there because it is poisonous and prevents peo- ....

\par ple from using the ethanol for drinking. This means that places like mgsljl\'e9tlily lin; YW"

Bpld lilp W'th a dark \'b0'|Y la!/G" at the b\'b0n\'b0m Qi

\par the giant hardware stores can carry gallons of cheap contami- be no ll ml cb IS pe GF

3ll1n\'b0rmaI\lquote Any S\'b0IV6"t mnt rnmmns wil

\par plated oihoho. oo many of yoo heve dieeoveied. the eieiiuei c/-~ Olwiofm if

,,f\'a7Z\'a7?\'a7g 'Q i,..i.g\lquote\'a7g"O?\'a7\lquote i\'a7i;?6.i\lquote i'hi?Z\'b0i;

'\'a7o?,31\ldblquote $oE,\'b0

\par be used 200mb of dark oily layer then a liter or more of water is pored in

\par and mixed really well. After things settle one will see a nice little

\par SO new that we have all the reagents out Of the way let'; see how l8yGI' of clear

lSOS3fl\rquote 0i\'80 fOfl'T'l Ht [l`l\'80 b0[[0lTl, 8 mLlfky bl'OWl\rquote l lyikes!

\par the reaction proceeds. There's the clear- yellow "safroIe" sitting in emulsion layer in the

middle and a blackish water layer on top.

\par the bottom if the flask and the clear saturated KOH solution is T|"l9 oil is Separated and theemulsion is dealt with in any way that

\par dumped in The solution is heated to reflux etc_ and yes, some is best from the below

mentioned strategies for emulsion tighting.

\par brown byproducts and destruction artifacts will appear, Especially This particular emulsion

is of very fine particulates and has a lot of

\par if the safrole is not pure. These byproducts should be expected to lsosafrole in it. lf one is

patient then one can add solvent (DCM is

\par some extent because concentrated basic (OH) solutions can be good) to the remaining

water/emulsion layer, shake then vacuum


34/246

\par as nasty as concentrated acidic solutions. One is mindful that filter. The crud remaining in

the filter is the junk that was causing

\par KOH is less intrusive towards the delicate methylenedioxy ring all the trouble. With it gone

one can now extract the remaining

\par structure ofthe safrole/lsosafrole molecule. water layer a couple more times with solvent,

add the solvent to

\par lhe isosafrole oil then remove the solvent by boiling or distillation

\par - \'a4 _ 0 \'b7

\par After 12-24 hours of reflux the reaction is, for the most part, com- O get pure lsosafrole ( 70

B0 /0 trans' 20 BDA, cls)

\par plete. The reaction mix will be a dark brown. So what does one do

\par about all those brown particles and junk. Well, usually there aren't NO-l-El a lcally goodoloooduro fol, bosllno up the omulslon

\par any- The Snlnnnn Snould be \{\'b7'n'f\'b0n`n|Y nant- if anY $\'b0l\lquote dS can be caused

by introducing the water is to slowly acidify the water layer

\par Seen 't means that tn\'80Y a\rquote\'80_'n$\'b0'\ldblquote b'E 'n etnnnnl and can be

\rquote\'b0' with HCI. As the water layer acidities one will see the emulsion

\par m\'a4v\'a4\'a4 frm ==\'b7\'a4l\'a4\'a4\'a4\'a4 bv \'a4r\'a4v\'b7tv \'a4n vacuum

tltr\'a4*\'b7\'a4\'a4 thi\'a4\'a4\'a4h \'a4


35/246

\par Sound easy? Well. preeedurelly ll le- But the yield eerl reelly e\'a4\'a4l< \'b7\'b7cA 47;9a60.

lsoearrole from earrore. yasnlnaru Ogata (Regen-

\par semellmes and lt een gel many messy. l-ele ef people have nel eration oampnar co). Japan.

5331 ('51), sep:. 15. Safrole

\par been pleased with lt. Strike wasn t. But what can you do? b_132_40, 100, CeO 15, end

KOH 1 g' are heeled 15 mln. at

\par Well, someone named Osmium sent Strike a journal reference 243\'b75O\'a4 the Ceo

a\rdblquote d KOH llllefed ell and the lillrefe disld fe \'a4b\'b7

\par about doing the exact procedure above but carrying it out in a mi- fain 95% isosafrole,

b.240-8\'b0. K. Kitsuta"

\par crowave [5]! A group of Brazilian folks tried both conventional and

\par ' ht'.Th hdt lh`h'ld llb . . , .

\par bggtlluveays. Seth SM asnlelautglile Iuwilgcorueilniraiitensaweug \lquote Not-Tlm said

Strike was wasting everybody's time wlthvthe etha-

\par used in ethanol, propanol and butanol, They also found that add- ug!/FQTH regpe end

Y\'b0u\'b7Wa"\rquote\ldblquote e knew What? He Wa$_k'"ua "9'lt

\par ing 2M KCI along with the KOH helped things. The really cool ( u' eee rezueu

Imerevememe ebeye elem hereluet te take

\par things were that when they used butanol and 4M KOH they only up $l\'b0"\'b0"\rquote\'b7)-

The '\ldblquote\'b0**\lquote\'b0u 'S S\'b0\'b0\'b0\'b0\'b0 east

\par dt l15' fb\lquote l` t t `ld f99\lquote VlS\lquote lth h . .

\par Isacteareseeny prorgarlllcj arcidnegzhgnge oewlyneleeiied 2?5h;lf0FgCg+; All one does IS

follow that CA reclpe to the letter. ln a small flat-

\par conversion. Strike would assume that the reduced reaction times b\'b0u\'b0u` flask pleee

1009 Sefrelel 159 CeO emu 19 New the

\par erlerded by The lereer elsehels end such may Very Well help re_ flask IS heated directly on

a stlrrlng hotplate (stlrrlng IS nlce but not

\par duce tar and destruction and make for a better procedure. ueeeeeeuu lf ene hee e

r\'b0u"u`b\'b0u\'b0m ueek er e lew Output heat`

\par lng source, a shallow oil bath can be employed to get even heat-

\par Uslne The mlereweve lusl decreased the reeellerl llme le 3_ ing. The really neat thing about

this method is the proof-positive

\par somlnules The dudes ln The erllele used e heuseheld 500W Bre_ heat gradations that will

occur. The mixture will rise to the boiling

\par Zlllen mlereweve (Ylkesl) They eel e whsle ln the lee el, the ml_ point of safrole (232-234\'b0C). And it will hold there for just a brief


36/246

\par ereweve le ellew the eerrderrser spperelus te pess through the second. Then it will start to

bubble and the temperature will rise!

\par oven. They then killed themselves most likely. But not before they Sur e e\'a4\'a4\'a4ell\'b7

eftei euly. 15mm ef the the temperature Wm reeeh

\par were able to scratch down this procedure as they slowly bumed to the ueer beumg umm ef

'eeeefrele ("243'25e C)\'b7 And that- ee they

\par seeth; say, IS lt.

\par TGENERAL PROCEDURE. The A/eehelie elkslme selrmen ls pre_ The oil that remains is

only slightly dark. Definitely translucent

\par pared by prolonged stirring of 8.8g (or 4.4g) of KOH pellets in xlzhlch is ehflzys

Ii?/ely\lquote dOue cer; lllgll ef? SOT; Weger le tekglgg

\par 30mL of alcohol. The alkaline solution is placed in a round\emdash boftom f e uueeee eb S;

ere; sepelge e e $0/rzuel ten euzul .5

\par flask provided with a reflux condenser (microwave or conventional Orme I can e Us e up

mu Some \'b0 \lquote e 'Sese lrzefl

\par systems). Then 4.0g of Safrole (or eugenol) is added and the so- clean eueugh

le \'a4r\'a4\'a4ee\'a4 Wuh but u een el eeuree be diem e or

\par rurlon neared? u te pu"*V\'b7

\par - 42 - - 43 -

\par

\par Strike can\rquote t believe ' - \'b7

\par All of the above isomerization recipes can, in theory, produce al- \{That is so freaky!)].

lli:>rsl;i\'a4f\'80t?1resae:tll1?ngsqvgilltgglgke5 gwn bP\'b0k\lquote

\par most 100% yields of isosafrole. But about 20-30% of that isosa\emdash that are much

more potent than X It is also sslnfbletamlnes

\par frole is in a screwed up configuration called 'cis'. This cis isomer around with some of the

little side grou s on the; il e to play

\par does not react the same way as trans and the drug that will be make X or some other

interesting psy\'a7hotomime$csO ellflimuauy

\par made from it will not be recognized in the same way as trans in exceptions these precursors

are all substituted all lbenz le few

\par the brain cells of USSFS. TSK. like safrole. They are all found in the same kind gf

legalggilg

\par /\\ O P O sold in the same kinds of places as sassafras. Finally, these pre-

\par cursors are turned into their own respective amphetamines using


37/246

\par O O the exact same conversion recipes used for safrole.

\par / / ANETHOLE: Up to_90+%4in anise seed oil, 70+% in fennel and

\par star anise oils, and in varying amounts in betel leaf, dill seed, car-

\par _ rot seed and coriander oils.

\par trans-isosafrole cis-isosafrole

\par H C

\par The chemist can try to separate the two isomers by careful frac- 3

\par tional distillation but it will be next to impossible to do because .

\par both the cls and the trans have practically the same boiling point. /

\par There are a few things that the chemist can do or hope for to get

\par rid of that cis isomer. The cis configuration is less stable than the

\par trans and may switch over to the trans configuration with a little

\par hel . The chemist can gentl heat the isosafrole oil to about

\par 150llC for an hour or so. Sheycan also try the same heating ex- ANl$ALDEl'lYDEl ln

Small 6l'\'a40\'a4\'a4fS (less than 5%) in anise,

\par cept have the oil mixed with some acetic acid. Also, the isosafrole \'b0"ln`lln\'b7 lennel end

slef afllse oils.

\par can be fractionally distilled to ultra purity and then be allowed to H CO

\par simply sit for a couple of days. Trans isosafrole \lquote may\rquote spontane- 3

\par ously crystalize out while the cis form remains as an oil. They can

\par then be separated by filtration. O

\par When all is said and done, the chemist may just wish to leave the _ ,, . _

\par damn cis isomer in with the trans. It's not really going to hurt g;lgl;]5`.23A\rdblquote jf

celeryleef \'b0ll* upl\'b0 3)% ln pelelelfleel and Seed

\par anything and if it goes unreacted in some of the conversion steps \rquote In sma am\'b0unls

ln \'b0ul\'b0eb\'b7 dlll end fennel Oile-

\par it will be lost in the process long before X is made. lt might even

\par correct itself during some of the conversion steps. /\\ O

\par O CH3

\par OTHER PRECURSORS

\par You people won't believe the potential amphetamine precursors H CO \\


38/246

\par just sitting around in naturally occurring oils and essential oils [6, 7 3 45

\par - 44 -

\par

\par ASARONE: 70-80% of calamus oil. ln trace amounts in Asian car- 5,:-O5\ldblquote :;I;:t,$n\'80?;\'a3?ts6gZ; Egemssgfgilfill and 'in Vawing

\par ~ . n various

\par mt Seed amd \'b0'\'b0V\'b0 bud \'b0'|s\'b7 amounts in fennel and carrot seed oils. Sma

\par HSCO CH3 /\\ O

\par / O

\par H3CO

\par BENZALDEHYDE: The precursor for speed. It makes up nearly HSCO \\

\par 100% of bitter almond oil. _Not a very popular oil with the DEA.

\par Some hints: Benzaldehyde is indispensable for the flavoring in- CH;

\par dustry. lt is the flavor in almond extract and .

\par synthetic benzaldehyde is used in all cherry ELEMICINT In V6l'Vl\'a49 \'a4lTl0\'a4\'a4T$

lll \'a4ltl\rquote 0\'a4\'80||9l \'80|\'80|T\\l. m6C\'80. nutmeg,

\par flavorings. Also, there is currently a little loop- Paisley $\'a4\'a4k\'80l\rquote 00\'a5 and

tafragon. \lquote

\par hole in the system when it comes to a product HO OCH

\par called \lquote Roasted Cassia Oil\rquote . Apparently, some \lquote 3

\par manufacturers take cassia oil and run it through some sort of in- H CO

\par dustrial process to change it into benzaldehyde. No one wanted to 3

\par tell Strike the particulars of how this was done. But one company

\par chemist gave me some hints (You can get really chatty with some \\

\par of these guys). HBCU

\par Apparently, these guys are taking regular old cassia oil and simply

\par running it through a series of distillations. This even happens in

\par the Asian fields when the oil is harvested so it obviously is not a EUGENOLZ |\'a4 VGFV

IHFQG amounts i\'a4 bay. \'a4i\'a4\'a4Bm0n, clove and

\par complicated process. Cassia oil is made up almost exclusively of pimento oils. ln goodly

amounts in basil. eucalyptus and tejpat.


39/246

\par cinnamaIdehyde.`Any of you girls have any idea what these com- Lots of trace amounts in

many other oils.

\par panies are doing to turn cheap cinnamaldehyde into benzalde- OCH

\par hyde'? Might be beneficial for you if you do. 3

\par CHAVICOL: Up to 20% in West Indian bay oil. HO

\par HO

\par \\

\par \\ METHYLCHAVICOL: Up to 80+% in most basil, chervil and fennel

\par oils. ln small amounts in star anise and wormwood.

\par - 46 - _ 47 _

\par

\par PHENYLACETIC ACID: Very important fragrance chemical. Only

\par H C recently was it banned by the DEA. Fragrance companies still

\par 3 can\lquote t believe they cannot openly sell it. It makes up 15% of jas-

\par mine oil (very expensive).

\par \\

\par METHYLEUGENOL: Up to 60% in various parts of the basil plant. COOH

\par Around 45% in snakeroot oil. In decent amounts in calamus, cas-

\par sie, myrtle, pimento, plstacia, pteronia and some forms of tarra-

\par gon . 2,3,4,5-TETRAMETHOXYALLYLBENZENE: In varying amounts

\par in some parsley oils (hell, just throw parsley oil in a pot to get a

\par OCH3 grab bag of psychedelic amphetamlnes!).

\par HECO OCH3

\par HSCO

\par \\

\par MYRISTICIN; ln moderate amounts in dill, carrot, celery, fennel, H CO \\

\par mace and nutmeg (no more than 10% tops). Makes up about 40% 3

\par of the oil of parsnip and can reach up to 50-60% of the oil of QQH3

\par parsley leaves and seeds. Give nutmeg a rest folks! It just don\rquote t


40/246

\par h\'a4V\'80 itwben Compared *0 P6V$l\'80Y 6\'a4\'a4l F>6FS\'a4\'a4P\'b7 VANILLIN: In

vanilla beans of course. But never more than 2%.

\par /\\ O This stuff is bought as a synthetic and is cheap and legal.

\par O CH3

\par HO

\par HSCO \\

\par _ _ _ HO

\par OSMORHIZOLE: Makes up 25% of the essential oll of chervll.

\par Very hard to rind this \'a4l|th0ugh. The standard way that scientists get these allylbenzenes

and

\par other goodies out of these oils is by careful, fractional distillation.

\par Haco CH3 You can see from above that some of the more desirable allylben-

\par zenes do not occur in high concentrations in the oils they are

\par found in. So that means there is a lot of crap one has to get rid of

\par \\ to isolate the goods. This is not as big of a concern as one might

\par think.

\par - 48 - \emdash 49 -

\par

\par sulfate intermediate with the elemicin causing it to migrate out of

\par Essential oils from plants are technically known as \lquote voIatile\lquote oils. the ell laYet

and Qc lntc the S\'a4lr\'a4r\'b7\'a4_e\'a4\'b7\'a4 la\'a7\rquote at- And Slhtie elemicin

\par -l-hls means, among olhel, thlngsl that most even, component of is goinglto be about the

only thing in elemi oil that has a terminal

\par them will eventually evaporate if left to stand. So there is a definite alkehe\'b7 't 's Qelhg re

hevahcut the \'b0nlV th'n9 that 9\'b0e$ into the aqid

\par boiling range for these oils which, compared to other things in na- laYet\'b7 P'eatO\'b7

Alkene 's\'b0lateu\'b7 Well. alnl\'b0$t- What the Ghemlet

\par ture, is relatively low. Strike means to say that when these oils eeee next la sePa'ate the aclu

lever (stlll cold mlnd V0Ul). Pl\'a4\'a4e lt

\par were extracted from the plants they come from, they were taken 'P SOmO Vessel and POut

lh a hlg Olu excess ef Watah The taht

\par by steam distillation where steam was the carrier. This leaves you getatute Wlll 9O uP anu

the hYut\'b09en sultate Wlll be ln$tahtlY hY\'b7


41/246

\par with compounds that have relatively low boiling points with 300\ldblquote C FO vzed PY

the Water tO_tOt!h ah Ol'l\'b7 One can else heat fer 5

\par being close to the max. And Strike can tell you right now that in mlhutOS re lhsute

OOh"etOlOh\'b7

\par oils that carry allylbenzenes, those same allylbenzenes are almost Wh t ,d _ _ _

\par always going to be the highest boiling compounds. Usually the _ a . happens [mug

,hydr\'b0lyS'S ls thatthe OH tOrma and the

\par bulk of the oil is constituted with compounds that boil well below Olem'O'h P'OPYl

alOOhOl u"OPs Out ef sclutlen and ferme tts \'b0Wn 0ll

\par the allylbenzenesl layer. Of course one won\rquote t see this because the solution is a big

\par old brown mess, lousy with emulsion particles. Emulsions suck!

\par People with or without distillation apparatuses can take advantage aut Oah be dealt WlthettectlVelV bv au\'a7?l'n9 a little acid Ol basal OF

\par of this fact. Just boil or distill off most of the oil up to the tempera- tllttatleh eee the lrke-

AhYWaY\'b7 atlet a llttle Walk UP Ona Qeta Some

\par ture of your preferred allylbenzene and stop. There is a very good teallY PU\'a4'e

Phenylpropyl compound. And if Strike had Strike s way,

\par ohanoe lhalwhal le lefl Will be a malorlly of what le Wahleo Strike would have that OH

stuck right on the middle (beta) carbon

\par of the species. Work could then progress on using that OH to get

\par -l-he above soooeellon le] of course, ralhel. loroaol lllloel oeoole an amphetamine (Sobl

Strike had so much about that subject that

\par would prefer a more specific solution. Unfortunately Strike has Stuke was PlèPalèdtO Put

lh thls backu-

\par one. For over half a year preceding this second edition Strike was _

\par pouring money and time into the realization of making an isopropyl Bur that_'s hOt the

eeee- What the Kctean lab found Out Was that

\par intermediate out of safrole using sulfuric acid (please don't ask). when thls PlOceuute ls

Pe'tOhheu\'b7 the OH stablllzes cn the @@1

\par So Strike hires this Korean research lab to work out the synthesis. ca'hOh\'b7 Ther la the

OalÒOh r\'b79r\'b7r_\'a4e>


42/246

\par henzeneo (Son olrl ohemloally our example). Using the simple potassium bisulfate

reductron

\par recipe, one can get rid of the OH with no problems at all.

\par The literature states that if one uses ice cold, concentrated sulfuric

\par aold oh a lermlhal alkehe la_l(_a_ allylhehzehel ah aloohol (OH) Hey! That really wasn't a

lot of work. Just a lot of talk on Strike's

\par intermediate will form \lquote MarkovnikovIy' on the secondary carbon Pau- All Ohe ulu

was mlx an err Wlth eeme aclu\'b7 auuecl water end

\par (ooh\'bbl aekl_ What does this meah? l_el\'b7a lake ah example. Say ohe isolated. One gets

some pure propenylbenzene without distillation.

\par has some elemi oil and wants that elemici

total synthesis ii strike.docx

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