Ppm


SD15.1D-DMSO-HMBC SD15.1-CDCl3+MeOD-HSQC



PL-25

6.5 6.0


5.5


5.0


4.5


4.0


ppm


136 137 138 139 140 141 5 PHỔ HSQC 142 143 144 145 146 147 148 149 150 151 152 153 154 155 ppm 9 1

136


137


138


139


140


141


5. PHỔ HSQC

142


143


144


145


146


147


148


149


150


151


152


153


154


155


ppm


9.0


8.5


8.0


7.5


7.0


6.5


6.0


5.5


5.0


4.5


4.0


3.5


ppm 40

45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 ppm SD15 1 2

45


50


55


60


65


70


75


80


85


90


95


100


105


110


115


120


125


130


135


140


145


150


155


160


ppm


SD15 1 CDCl3 MeOD HSQC ppm 100 105 110 115 120 125 130 135 140 SD15 1D DMSO HSQC ppm 30 40 50 60 70 3

SD15.1-CDCl3+MeOD-HSQC


ppm


100


105


110


115


120


125


130


135


140

SD15.1D-DMSO-HSQC


ppm


30


40


50


60


70


PL-26

80


90


100


110


120


130


140


150



8.0 7.8


7.6


7.4


7.2


7.0


6.8


6.6


6.4


6.2


ppm


8.0


7.5


7.0


6.5


6.0


5.5


5.0


4.5


4.0


3.5


3.0


2.5

160


ppm SD15 1D DMSO HSQC ppm 100 105 110 115 120 125 130 135 140 PL 27 7 8 7 6 7 4 7 2 7 0 6 8 6 6 6 4 4

ppm


SD15 1D DMSO HSQC ppm 100 105 110 115 120 125 130 135 140 PL 27 7 8 7 6 7 4 7 2 7 0 6 8 6 6 6 4 ppm 5

SD15.1D-DMSO-HSQC


ppm


100


105


110


115


120


125


130


135


140



PL-27

7.8 7.6


7.4


7.2


7.0


6.8


6.6


6.4


ppm

Phụ lục 3.3. Hợp chất SD3: oxostephanin

CTPT: C18H11NO4 M = 305

Chất bột vô định hình màu vàng cam


1 H NMR 500 MHz DMSO d 6 13 C NMR 125 MHz DMSO d 6 DEPT COSY HMBC HSQC 1 PHỔ 1 H NMR 8 715 8 704 6

1H-NMR (500 MHz, DMSO-d6)

13C-NMR (125 MHz, DMSO-d6)

DEPT COSY HMBC HSQC


1. PHỔ 1H-NMR


8.715

8.704

8.210

8.194

7.875

7.865

7.712

7.696

7.680

7.405

7.239

7.222

6.412

3.952

SD01-DMSO-1H


3 069 2 507 2 504 2 500 2 496 2 493 0 008 Current Data Parameters NAME DUNG SD01 EXPNO 1 PROCNO 1 7


3 069 2 507 2 504 2 500 2 496 2 493 0 008 Current Data Parameters NAME DUNG SD01 EXPNO 1 PROCNO 1 8

3.069

2.507

2.504

2.500

2.496

2.493

0.008

Current Data Parameters NAME DUNG_SD01

EXPNO 1

PROCNO 1

F2 - Acquisition Parameters Date_ 20201023

Time 8.47

INSTRUM spect PROBHD 5 mm PABBO BB/ PULPROG zg30

TD 65536

SOLVENT DMSO

NS 16

DS 2

SWH 10000.000 Hz

FIDRES 0.152588 Hz

AQ 3.2767999 sec

RG 111.09

DW 50.000 usec

DE 6.50 usec

TE 353.0 K

D1 1.00000000 sec

TD0 1

======== CHANNEL f1 ======== SFO1 500.2420892 MHz NUC1 1H

P1 10.20 usec

PLW1 22.00000000 W

SI SF WDW

SSB


0

65536

500.2390042 MHz

EM

LB


0.30 Hz

GB

0


PC


1.00

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F2 - Processing parameters


1.00

1.01

1.04

1.06

0.98

1.06

2.13

3.13

13 12 11 10 9 8 7 6 5 4 3 2 1 0 -1 ppm

8 715 8 704 8 210 8 194 7 875 7 865 7 712 7 696 7 680 7 405 7 239 7 222 SD01 DMSO 1H 1 00 1 01 1 04 15

8.715

8.704

8.210

8.194

7.875

7.865

7.712

7.696

7.680

7.405

7.239

7.222

SD01-DMSO-1H




1 00 1 01 1 04 1 06 0 98 1 06 8 8 8 7 8 6 8 5 8 4 8 3 8 2 8 1 8 0 7 9 7 8 7 7 7 6 7 5 7 4 7 3 7 2 22


1.00

1.01

1.04

1.06

0.98

1.06

8.8 8.7

8.6

8.5

8.4

8.3

8.2

8.1

8.0

7.9

7.8

7.7

7.6

7.5

7.4

7.3

7.2

ppm


2. PHỔ 13C-NMR


179.69

160.86

151.22

147.37

145.77

143.77

134.47

134.26

134.19

122.90

121.05

120.22

118.83

112.70

106.73

102.59

102.40

55.84

40.00

39.83

39.66

39.50

39.33

39.16

39.00

SD01-DMSO-C13CPD



Current Data Parameters NAME DUNG_SD01

EXPNO 2

PROCNO 1

F2 - Acquisition Parameters Date_ 20201023

Time 9.12

INSTRUM spect PROBHD 5 mm PABBO BB/

PULPROG zgpg30

TD 65536

SOLVENT DMSO

NS 256

DS 4

SWH 31250.000 Hz

FIDRES 0.476837 Hz

AQ 1.0485760 sec

RG 198.57

DW 16.000 usec

DE 6.50 usec

TE 353.0 K

D1 2.00000000 sec

D11 0.03000000 sec

TD0 1

======== CHANNEL f1 ======== SFO1 125.7990330 MHz NUC1 13C

P1 10.00 usec

PLW1 88.00000000 W

======== CHANNEL f2 ======== SFO2 500.2410010 MHz NUC2 1H

CPDPRG[2 waltz16

PCPD2 80.00 usec

PLW2 22.00000000 W

PLW12 0.35764000 W

PLW13 0.17989001 W

SI SF WDW

SSB


0

32768

125.7853110 MHz

EM

LB


1.00 Hz

GB

0


PC


1.40

F2 - Processing parameters


220 200 180 160 140 120 100 80 60 40 20 0 ppm 180 135 134 47 170 134 26 160 130 134 19 150 140 130 36

220 200 180 160 140 120 100 80 60 40 20 0 ppm



180 135 134 47 170 134 26 160 130 134 19 150 140 130 SD01 DMSO C13CPD 125 122 90 121 05 120 120 120 37

180 135 134 47 170 134 26 160 130 134 19 150 140 130 SD01 DMSO C13CPD 125 122 90 121 05 120 120 120 38

180

135

134.47

170

134.26

160

130

134.19


150

140

130

SD01-DMSO-C13CPD

125

122.90


121.05

120

120

120.22


110

118.83


100

90

115

110

112.70


80

106.73

70

60

105

102.59

ppm

ppm

102.40

179.69


160.86


SD01-DMSO-C13CPD

151.22

147.37

145.77

143.77


134.47

134.26

134.19


PL-30

122.90

121.05

120.22

118.83


112.70


106.73

102.59

102.40



55.84

3. PHỔ DEPT



DEPT90

SD01-DMSO-C13CPD&DEPT



210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 ppm DEPT135 CH CH3 CH2 61

210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 ppm

DEPT135


CH CH3 CH2 210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 ppm C13CPD 62

CH&CH3 CH2


210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 ppm C13CPD 210 200 190 64

210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 ppm

C13CPD


210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10 ppm



DEPT90

SD01-DMSO-C13CPD&DEPT



145 DEPT135 140 135 130 125 120 115 110 105 100 95 90 85 80 75 70 65 60 ppm CH CH3 CH2 145 C13CPD 65

145

DEPT135

140

135

130

125

120

115

110

105

100 95 90

85 80

75 70

65 60

ppm


CH CH3 CH2 145 C13CPD 140 135 130 125 120 115 110 105 100 95 90 85 80 75 70 65 60 ppm 145 140 135 66

CH&CH3 CH2


145

C13CPD

140

135

130

125

120

115

110

105

100 95 90

85 80

75 70

65 60

ppm


145 140 135 130 125 120 115 110 105 100 95 90 85 80 75 70 65 60 ppm 4 PHỔ COSY ppm 2 5 3 0 3 5 4 68

145 140

135

130

125

120

115

110

105

100 95

90 85 80

75 70

65 60

ppm

4. PHỔ COSY


ppm


2.5


3.0


3.5


4.0


4.5


5.0


5.5


6.0


6.5


7.0


SD01-DMSO-COSYGP



Current Data Parameters NAME DUNG SD01 EXPNO 7 PROCNO 1 F2 Acquisition Parameters Date 20201023 69

Current Data Parameters NAME DUNG SD01 EXPNO 7 PROCNO 1 F2 Acquisition Parameters Date 20201023 70

Current Data Parameters NAME DUNG_SD01

EXPNO 7

PROCNO 1

F2 - Acquisition Parameters Date_ 20201023

Time 9.04

INSTRUM spect PROBHD 5 mm PABBO BB/

PULPROG cosygpppqf TD 2048

SOLVENT DMSO

NS 2

DS 8

SWH 5000.000 Hz

FIDRES 2.441406 Hz

AQ 0.2048000 sec

RG 64.21

DW 100.000 usec

DE 6.50 usec

TE 353.0 K

D0 0.00000300 sec

D1 2.00000000 sec

D11 0.03000000 sec

D12 0.00002000 sec

D13 0.00000400 sec

D16 0.00020000 sec

IN0 0.00020000 sec


======== CHANNEL f1 ======== SFO1 500.2412511 MHz

NUC1 1H

P0 10.20 usec

P1 10.20 usec

P17 2500.00 usec

PLW1 22.00000000 W

PLW10 2.54320002 W


====== GRADIENT CHANNEL ===== GPNAM[1] SMSQ10.100

GPZ1 10.00 %

P16 1000.00 usec


F1 - Acquisition parameters TD 160

SFO1 500.2413 MHz

FIDRES 250.000000 Hz

SW 9.995 ppm

FnMODE QF

7.5


8.0


8.5


9.0

9 8 7


6 5 4 3


ppm

F2 - Processing parameters SI 1024

SF 500.2390000 MHz

WDW QSINE

SSB 0

LB 0 Hz

GB 0

PC 1.00

F1 - Processing parameters SI 1024

MC2 QF

SF 500.2390000 MHz

WDW QSINE

SSB 0

LB 0 Hz

GB 0


ppm


7.2


SD01-DMSO-COSYGP


Current Data Parameters NAME DUNG SD01 EXPNO 7 PROCNO 1 F2 Acquisition Parameters Date 20201023 71

Current Data Parameters NAME DUNG SD01 EXPNO 7 PROCNO 1 F2 Acquisition Parameters Date 20201023 72

Current Data Parameters NAME DUNG_SD01

EXPNO 7

PROCNO 1

F2 - Acquisition Parameters Date_ 20201023

Time 9.04

INSTRUM spect PROBHD 5 mm PABBO BB/

PULPROG cosygpppqf TD 2048

SOLVENT DMSO

7.4

7.6

NS 2

DS 8

SWH 5000.000 Hz

FIDRES 2.441406 Hz

AQ 0.2048000 sec

RG 64.21

DW 100.000 usec

DE 6.50 usec

TE 353.0 K

D0 0.00000300 sec

D1 2.00000000 sec

D11 0.03000000 sec

D12 0.00002000 sec

D13 0.00000400 sec


7.8


8.0

D16 0.00020000 sec

IN0 0.00020000 sec


======== CHANNEL f1 ======== SFO1 500.2412511 MHz

NUC1 1H

P0 10.20 usec

P1 10.20 usec

P17 2500.00 usec

PLW1 22.00000000 W

PLW10 2.54320002 W


====== GRADIENT CHANNEL ===== GPNAM[1] SMSQ10.100

GPZ1 10.00 %

8.2

P16

1000.00 usec


8.4


8.6


8.8


8.8


8.6


8.4


8.2


8.0


7.8


7.6


7.4


7.2


ppm

F1 - Acquisition parameters TD 160

SFO1 500.2413 MHz

FIDRES 250.000000 Hz

SW 9.995 ppm

FnMODE QF


F2 - Processing parameters SI 1024

SF 500.2390000 MHz

WDW QSINE

SSB 0

LB 0 Hz

GB 0

PC 1.00


F1 - Processing parameters SI 1024

MC2 QF

SF 500.2390000 MHz

WDW QSINE

SSB 0

LB 0 Hz

GB 0

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