busra arvas, *omer tahir gunkara, and nuket ocal

24
General Papers ARKIVOC 2018, vii, S1-S24 Page S1 © ARKAT USA, Inc Supplementary Material Synthesis of arylpiperazine substituted bisindolylmethanes as possible pharmacologically active new compounds Busra Arvas, Omer Tahir Gunkara, and Nuket Ocal * Yildiz Technical University, Faculty of Science and Arts, Department of Chemistry, Davutpasa Campus, 34220, Esenler, Istanbul, Turkey Email: [email protected] Table of Contents New bisindolylmethanes list ...................................................................................................................... S2-S4 IR, 1H-NMR, 13C-NMR, Qtof or LCMS spectra of new compounds .......................................................... S5-S24

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Page 1: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S1 ©ARKAT USA, Inc

Supplementary Material

Synthesis of arylpiperazine substituted bisindolylmethanes as possible pharmacologically active new compounds

Busra Arvas, Omer Tahir Gunkara, and Nuket Ocal *

Yildiz Technical University, Faculty of Science and Arts, Department of Chemistry, Davutpasa Campus, 34220,

Esenler, Istanbul, Turkey Email: [email protected]

Table of Contents

New bisindolylmethanes list ...................................................................................................................... S2-S4

IR, 1H-NMR, 13C-NMR, Qtof or LCMS spectra of new compounds .......................................................... S5-S24

Page 2: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S2 ©ARKAT USA, Inc

Entry Compound Name Compound Structure

3 3,3’-((4-Chlorophenyl)methylene)bis(1-(4-

bromobutyl)-1H-indole)

4 3,3’-((4-Fluorophenyl)methylene)bis(1-(4-

bromobutyl)-1H-indole)

5 3,3’-(Phenanthren-9-ylmethylene)bis(1-(4-

bromobutyl)-1H-indole)

6 3,3’-(Naphthalen-2-ylmethylene)bis(1-(4-

bromobutyl)-1H-indole)

11 1-(4-Bromobutyl)-3-((4-chlorophenyl)(1-(4-

(4-(2,3-dichlorophenyl)piperazin-1-yl)butyl)-

1H-indol-3-yl)methyl)-1H-indole

Page 3: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S3 ©ARKAT USA, Inc

12

1-(4-Bromobutyl)-3-((1-(4-(4-(2,3-

dichlorophenyl)piperazin-1-yl)butyl)-1H-

indol-3-yl)(phenanthren-9-yl)methyl)-1H-

indole

13

1-(4-Bromobutyl)-3-((1-(4-(4-(2,3-

dichlorophenyl)piperazin-1-yl)butyl)-1H-indol-3-yl)(naphthalen-2-yl)methyl)-1H-

indole

14 1-(4-Bromobutyl)-3-((4-chlorophenyl)(1-(4-

(4-(pyrimidin-2-yl)piperazin-1-yl)butyl)-1H-

indol-3-yl)methyl)-1H-indole

15 1-(4-Bromobutyl)-3-((4-fluorophenyl)(1-(4-

(4-(pyrimidin-2-yl)piperazin-1-yl)butyl)-1H-

indol-3-yl)methyl)-1H-indole

Page 4: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S4 ©ARKAT USA, Inc

17 3,3’-(Phenylmethylene)bis(1-(4-(4-(3-

8trifluoromethyl)phenyl)piperazin-1-

yl)butyl)-1H-indole

Page 5: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S5 ©ARKAT USA, Inc

Compound 3

IR Spectrum of Compound 3

1H NMR spectrum of Compound 3

52

6.2

65

38

.67

56

0.4

95

71

.20

59

1.1

96

46

.25

67

1.8

67

02

.73

73

6.9

87

98

.80

85

9.2

19

25

.60

96

2.1

61

01

3.4

91

04

1.0

81

08

8.1

31

12

2.7

11

15

5.3

611

99

.80

12

18

.73

12

51

.57

12

63

.74

13

34

.01

13

59

.16

13

93

.40

14

65

.86

14

87

.58

15

47

.12

16

11

.25

17

32

.71

19

77

.54

20

32

.092

16

0.0

8

28

72

.18

29

37

.60

30

46

.16

BD-7 2-14 arasi

30

35

40

45

50

55

60

65

70

75

80

85

90

%T

1000 1500 2000 2500 3000 3500 4000

Wavenumbers (cm-1)

Page 6: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S6 ©ARKAT USA, Inc

13C NMR spectrum of Compound 3

QTof Spectrum of Compound 3

Page 7: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S7 ©ARKAT USA, Inc

Compound 4

IR spectrum of Compound 4

1H-NMR spectrum of Compound 4

60

6.2

46

38

.156

71

.80

73

7.3

37

83

.84

80

5.4

88

57

.269

26

.21

95

9.6

91

01

3.6

91

03

7.4

61

09

2.7

01

12

2.6

81

15

4.1

41

21

6.6

11

25

2.0

51

29

2.5

01

33

4.3

31

36

0.6

513

93

.57

14

65

.81

14

79

.47

15

04

.31

15

47

.05

16

01

.52

16

68

.09

17

09

.21

19

78

.46

20

34

.13

21

60

.81

28

51

.63

29

22

.99

30

46

.76

bd11t

60

65

70

75

80

85

90

95

%T

1000 1500 2000 2500 3000 3500 4000

Wavenumbers (cm-1)

Page 8: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S8 ©ARKAT USA, Inc

APT spectrum of Compound 4

LCMS Spectrum of Compound 4

Page 9: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S9 ©ARKAT USA, Inc

Compound 5

IR spectrum of Compound 5

1H-NMR spectrum of Compound 5

61

5.8

06

61

.22

70

1.2

47

28

.85

74

7.5

17

96

.03

86

4.4

291

0.8

11

01

5.3

410

81

.6112

58

.99

13

36

.61

13

62

.161

39

5.3

71

44

6.0

31

46

5.2

11

54

5.2

91

61

0.0

41

65

4.1

017

24

.30

19

78

.46

20

29

.00

21

61

.02

28

51

.53

29

21

.17

29

61

.62

bd14t

45

50

55

60

65

70

75

80

85

90

95

%T

1000 1500 2000 2500 3000 3500 4000

Wavenumbers (cm-1)

Page 10: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S10 ©ARKAT USA, Inc

13C NMR spectrum of Compound 5

LCMS Spectrum of Compound 5

Page 11: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S11 ©ARKAT USA, Inc

Compound 6

IR spectrum of Compound 6

1H-NMR spectrum of Compound 6

73

9.1

47

66

.27

77

8.6

28

04

.07

83

0.9

68

48

.89

86

2.7

49

00

.26

90

9.9

29

28

.33

94

8.0

79

61

.83

10

10

.85

10

30

.80

10

43

.10

10

71

.67

10

96

.82

11

25

.42

11

55

.18

11

70

.81

11

96

.31

12

20

.12

12

48

.41

12

69

.22

12

90

.78

13

33

.04

13

59

.80

13

95

.80

14

34

.93

14

44

.12

14

66

.80

14

78

.92

15

06

.32

15

49

.421

60

1.1

31

61

0.8

316

32

.79

16

47

.13

17

30

.72

17

68

.42

18

88

.12

19

22

.39

19

78

.31

20

28

.29

21

60

.81

28

77

.30

29

40

.74

30

48

.41

31

26

.42

BD15

50

55

60

65

70

75

80

85

90

95

%T

1000 1500 2000 2500 3000 3500 4000

Wavenumbers (cm-1)

Page 12: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S12 ©ARKAT USA, Inc

APT spectrum of Compound 6

LCMS Spectrum of Compound 6

Page 13: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S13 ©ARKAT USA, Inc

Compound 11

IR Spectrum of Compound 11

1H-NMR spectrum of Compound 11

64

8.2

46

72

.12

71

3.7

07

33

.71

78

0.6

28

00

.21

85

9.6

59

07

.28

96

1.0

71

01

3.7

01

04

4.5

61

05

8.8

21

08

8.2

11

10

1.3

51

13

7.1

11

15

4.9

711

99

.48

12

40

.36

12

82

.17

13

34

.38

13

64

.38

13

93

.81

14

21

.23

14

47

.05

14

65

.63

14

87

.66

15

48

.22

15

77

.15

16

11

.65

17

14

.92

19

79

.24

21

61

.14

22

42

.90

28

18

.77

28

73

.29

29

32

.03

30

47

.34

BD-8 tekrar

30

35

40

45

50

55

60

65

70

75

80

85

90

%T

1000 1500 2000 2500 3000 3500 4000

Wavenumbers (cm-1)

Page 14: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S14 ©ARKAT USA, Inc

APT spectrum of Compound 11

QTof spectrum of Compound 11

Page 15: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S15 ©ARKAT USA, Inc

Compound 12

IR spectrum of Compound 12

1H-NMR spectrum of Compound 12

61

6.9

46

29

.64

64

4.8

16

71

.92

71

3.5

67

26

.69

74

0.3

27

80

.86

82

4.0

89

05

.87

95

8.1

11

01

3.2

41

04

3.8

5

11

36

.29

11

54

.64

11

68

.78

12

00

.39

12

39

.83

13

03

.40

13

35

.22

13

63

.03

14

21

.86

14

48

.41

14

65

.16

14

94

.28

15

49

.79

15

77

.5216

11

.29

16

75

.70

17

32

.23

19

77

.81

20

28

.42

21

60

.15

23

23

.74

28

50

.79

29

22

.01

30

52

.89

33

35

.88

BD-16

86

87

88

89

90

91

92

93

94

95

96

97

98

%T

1000 1500 2000 2500 3000 3500

Wavenumbers (cm-1)

Page 16: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S16 ©ARKAT USA, Inc

APT spectrum of Compound 12

QTof Spectrum of Compound 12

Page 17: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S17 ©ARKAT USA, Inc

Compound 13

IR spectrum of Compound 13

1H-NMR spectrum of Compound 13

61

8.9

66

46

.75

67

3.4

57

11

.86

73

8.2

57

66

.41

77

8.4

78

06

.52

86

3.5

29

23

.3894

5.5

39

61

.54

10

12

.831

04

3.5

811

36

.46

11

83

.35

12

40

.41

14

08

.14

15

72

.04

19

77

.65

20

33

.97

21

60

.58

28

50

.80

29

26

.45

30

01

.71

33

34

.61

BD-17

20

25

30

35

40

45

50

55

60

65

70

75

80

85

90

95

%T

1000 1500 2000 2500 3000 3500

Wavenumbers (cm-1)

Page 18: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S18 ©ARKAT USA, Inc

APT spectrum of Compound 13

QTof Spectrum of Compound 13

Page 19: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S19 ©ARKAT USA, Inc

Compound 14

IR spectrum of Compound 14

1H-NMR spectrum of Compound 14

73

7.5

27

95

.89

86

0.4

79

35

.61

95

6.7

99

82

.511

01

3.2

71

03

9.7

21

08

7.8

01

12

1.9

41

15

3.1

81

17

3.7

91

23

9.9

21

25

7.5

41

28

5.8

11

30

6.5

11

33

3.6

51

35

7.6

81

39

1.5

11

44

5.3

91

46

6.3

01

48

7.5

81

54

5.6

01

58

3.7

01

61

0.9

0

17

32

.66

19

77

.44

20

29

.51

21

60

.29

28

10

.28

28

52

.19

29

27

.37

30

45

.11

32

66

.87

BD10

78

80

82

84

86

88

90

92

94

96

98

100

%T

1000 1500 2000 2500 3000 3500 4000

Wavenumbers (cm-1)

Page 20: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S20 ©ARKAT USA, Inc

APT spectrum of Compound 14

MS Spectrum

QTof Spectrum of Compound 14

Page 21: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S21 ©ARKAT USA, Inc

Compound 15

IR spectrum of Compound 15

1H-NMR spectrum of Compound 15

73

7.1

47

83

.30

79

6.6

18

34

.52

86

3.7

39

56

.58

98

2.5

910

13

.89

10

43

.17

10

84

.17

11

21

.07

11

53

.75

11

74

.21

12

17

.90

12

57

.42

12

91

.16

13

06

.92

13

34

.88

13

57

.58

13

91

.98

14

45

.99

14

66

.33

14

80

.39

15

04

.61

15

46

.27

15

83

.99

17

32

.49

19

77

.95

20

30

.73

21

60

.57

28

10

.85

28

53

.23

29

32

.9930

45

.99

33

69

.10

BD-12

25

30

35

40

45

50

55

60

65

70

75

80

85

90

95

%T

1000 1500 2000 2500 3000 3500 4000

Wavenumbers (cm-1)

Page 22: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S22 ©ARKAT USA, Inc

APT spectrum of Compound 15

QTof Spectrum of Compound 15

Page 23: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S23 ©ARKAT USA, Inc

Compound 17

IR spectrum of Compound 17

1H-NMR spectrum of Compound 17

53

1.4

55

50

.55

60

3.5

16

67

.90

69

5.0

874

0.9

07

82

.17

82

4.2

88

48

.46

94

8.8

79

91

.93

10

44

.48

10

75

.73

11

21

.3311

82

.43

12

33

.22

12

89

.51

13

09

.35

13

50

.27

14

52

.0514

94

.14

16

09

.96

16

98

.96

20

30

.29

21

61

.02

23

59

.37

29

23

.49

29

66

.53

J-232

40

45

50

55

60

65

70

75

80

85

90

95

100

105

%T

1000 2000 3000 4000

Wavenumbers (cm-1)

Page 24: Busra Arvas, *Omer Tahir Gunkara, and Nuket Ocal

General Papers ARKIVOC 2018, vii, S1-S24

Page S24 ©ARKAT USA, Inc

APT spectrum of Compound 17

QTof Spectrum of Compound 17