c3 mnr and xray
TRANSCRIPT
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8.58. 0
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HandoutPor8G170?9r antc FTI NMI.I,\[PORTANTF,orabgroupshonoedosubmitoRvIAL BFBORTpleasenclude nswe$othet:l*gul
bonusquest ellg*tggIR SpectroscoPY:
l. CanIR spectxoscopy e used ot utt tinOt pf * t"t$ffi
*l tffilTJff$*ose ofapplyingmagneticietd uringMR pectroscopv?2. Discuss bout2 factors hatcan.orrt lbut" to theshieldingn H-NMR'
Info source:httP l/www,chem'uqal . ca/cour$_es/3o/carey/qh13 ffi
r Involvesheexcitationof bond vibrationswithin thatmoleculeby absorption f infrared adiation'Vibrationsnclude tretchingmd hendingmodes'. Usually plitan R spechumntotwo approxlryrateegions:
nfra-Red ectrosco
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2. For heavieratoms.attached larger k value), u clecreases.Asexampresf his,norcreriiiiunrir{r"rroruiiiirrcomparc:C-H 3000m-r)C-C 1000m-r)C-Ct S00 m-r)
fihcuftelre {qto
t|rm tgolEtnp.rnurbans /crr-l'l' ,'
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tthlDbrnlsog.ClCclN
ft$tbnralsi l torbb Ibordr 1JJF'o-nl()'C I
mlro w aDsorpuonsBase StrengthIi rtil ti
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tH"
+ffft ffigm*ByntlI t t l l -t f ,a taII I I+ Ntlr l lTXIIIEt l l lv otIAII
d'ifiBfr. , , . . tr tlal
?TIITT.-rr.H{Fl-FFtttlr t
ttfft-+fi+FLowmffsr 1-&ssxqdiab*-- -*---*--: --- ---------**-*-*Ground$rtg _.-* **-* I{EHLTEIE--_* * ** *--:-=:=:;--'---":-.-=tup-tutasonfrlstren^4lt{^T::fr{A*"etiefr 'etd'Itisusuallvsmatfwrdiorrespondso the radiofrequencytange of theEM spectrum'silrua, qN wt. etl'v.a\stonger magneticield increas* Gyn*utiqn of-e:rergies f thespin states, ndthereforesodoes henequJncyequiiedocausehespin-flip'only EMenergy quivalento theenergy ifference etweenhenuclear pinstateswill beabsorbedthustheterm"Feasonance".
Ipterp,rettingIH'NMR SI ectrqIIow many ypesof H ?What typesof H ?
To* manyH of each YPeare there?
Indicated y howmanygroups f signalsherearen thespechaIndicatedy thechemicalhift(6)ot each roupIndicate
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c Tlteareaof opeak isproportion l to thenwnbe, of E tbathepeak epresenrs The ntegralmeasuresheareaof thepeakand giuo trr. rehtivi rotioif thenumber f H for eachpeakCoupling##ffi:T. t- "o -pJ 9t:i :-g.sletu-ep. elslbessrs".sbessfpns,.sssssgthe-nsrelxg-Alsoknownassignalmultiplicity or splitting.
--.- 4le*pls
fntegration
Based ntheoutlinegivenabove he bur setsof informationwe getare: ' 0 ppmr J basiclpesof H presentn the atioof 5 :2 : 2 :2 :3.
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acefyl'sali,cYlate
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Sal icyl ic Acid 1H NMR
11 10t li=l
\oooctla o\\o\qOf-o\cac.i
p-r lJ') tf) -r f- CA O\ O (l) C-. tf, cn \Or- \f oo oo tn cf) c{ oo rn (\l o\ \o \f, c\tO\ O\ rn (n tn rn tn C\ c, c' cl\ c|\ cr\ Cr\C- [*- f- [.- f- t-l. [-- f- [-- f- \O \O aO \ONt/ / , , , ,
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Current Data ParametersNAI,{E Sal icyl ic AcidEXPNO 44PROCNO 2F2 Acquisi t ion ParametersDate 2005082 4Time- 11- 33INSTRUM spectPROBHD 5 mm PABBO BB-PULPROG zg30TD 65536SOLVENT CDCI3NS 1DS OSt{H 6172 .839 HzFIDRES 0.094190 HzAQ 5.3084664 se cRG 25 6DW 81.000 usecDE 6.00 usecTE 296 .5 KDl 1.00000000 se cTDO 1:=:=,====NUCP1PL lSFO l
CHANNEL 1 =:====::1H8 .50 usec-3.00 dB300.1"318534 MH z?2SISF90DWSS BLBGBPC
Processing parameters327 68300. 1300000 MH zno00.00 Hz0i .00
7654321ppmf=l=lI
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CBE, 2nd ear
Synthesisand chara ctertzationof aspirin
Thereaction:
Figure1:NMRSpectraf salicylicacid,aspirinandarepresentativetudentproduct '
roH \ ,OHl_^,qi9,*l.9?tlLYqrl$P, p\fo*r'$HuV8$aficyllcasid acetylsalricyli,ccid
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r,Ia
122 Nuclear Magrletic ResonanceSpectroscopy Part One: Basic ConceptsTABLE 3.4APPROXIMATE HEMICAT HIFTRANCESPPM)FORSETECTEDYPES F PROTONSAR-CH3R-CH3-RR3CH
0.7 L.31.2 1.41.4 7.7
IR_N-C_Hll ,IR_S-C-HI
II*C-HI
IBr-C-HIICI-C-HI
of tlR-S-O-C*Hil lot lRO-C-Ir. HO-C-Ht l
ioil tR-C-O-C-HI
2.2 2.9
2.4 3.0
2.4 4.0
2.7 4.1
3.1 4.1
ca.3.0
3.2 3.8
3.5 4.8
ooi l t fl lR-C-C-H, H-C-C-Hflooi l t tf lRO-C-q-H, HO-C-C-Hll
tl lR-C:C-C-HI
1.6 2.6
2,r 2. 4
2.1 2.s
2.1 3.0'o
. | ; . . .4.2.3 2.7Ic-EI
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Date:8l26l2005Time::15:10 Mcm-1800000404
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Name: Yew ChuanF\:fn. 1a 1n .)n1?VOLU. LL. lV. LW LJGroup No. : 15slolF.-1 OrO@C{r{LOLOOOrJ r-l r-l r-l \O \O \g (tO =if' siF Cn Ol OO N 11 r-{ r{ r-{
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Date'r'].meINSTRUMPUTPROGTDSOLVENTNSDSSWHFI DRESAQRGDWDETED1TD O
NUC 1P1PL 1SFOl
z93055536CDCl3I626712.839 Hz0. C94190 Hz5. 30 84660 se cB12 .' l81.000 usec6.00 usec296.6 K1.00000000 se c1F1Ll- 1H9.10 usec-3.00 dB
\r W8.0 7"8 7.6 7.&
r\ L: A \1\T El T\- I rl-\l \ l \ IJ
3C0.l-318534 MH zF2 Processi-ng parameterssr 321 68SF 300.1300000 MH zWDW NOSSB CLB 0.00 HzGB OPC 1.00
3ilsl#lilr *
'fx fiii
ls l ilvii xli f f i iat*Yhr i*\ ;\ie iq iql t \ i iq ii f f iF ft$ f f iF if f i i i {p i
1& t3 12, ts ppm
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NiamelJ.= 1- cr ./r4\?\_,.
aCetyl .*5ai :-cyi :c ecj-d22. i0.2CL3G cuc ldc . :Ol ana{ i-- ss@6rrF-Ct(\a C\ f-- j ) .J)mN\if ' .$\ i"$jCO>
r- r-- ri r-{ \C \g (-C \iJ S s:' (-l 3l r.-r r{ r-i r-i r-i
li irililI t , { | il*-t--J
:**ia il c l i'a o |l;t=+)iq i iq ii r - : i c} i
lr - {- ,riJd. Lg'.i"'j-ineINSTRUMPROtsHPUtPR.OGTNSCi,VANTt\ f i
ilSq tii FirI DRNSaQDWDETTDiTD O .,1 f lf \ "i\ UL. .LP1] .1 t 5
SFOi
: r i3 i0t0l .6. . l -0sPect5 irun PABIIQ BB-zg3065536CNCI3i62'r ,3.12.839F'^z). S94190 Hz5.3084660 se c36 281.0006. 00296.6i . cc00000c
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usecus ecse c
t l - iAl;NEt f I ==:==*:::*1H9. 70 usec-3. 00 dB3i lc. i318534 Ml iz,i t i Il i i lvtJ UL
:tSISTWD Wi )b11LtsGE
Frc'cess nE paraneters32768300. i300000 MH znr\llv
t"\UC.00 Hz
t\V1 n /-\r. UU.6 7. 4 ppm
1, I s,i*i i*ti* * i iviiqe * i
32frr,,,,Jh)is in-* l#iic is. i i t : l i
t4 r3 12 10 pp m
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