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4. PHỔ COSY


ppm


SD08-DMSO-COSYGP



Current Data Parameters NAME 11THAO SD08 EXPNO 7 PROCNO 1 F2 Acquisition Parameters Date 20200421 1

Current Data Parameters NAME 11THAO SD08 EXPNO 7 PROCNO 1 F2 Acquisition Parameters Date 20200421 2

Current Data Parameters NAME 11THAO_SD08

EXPNO 7

PROCNO 1

F2 - Acquisition Parameters Date_ 20200421

Time 18.30

TD

2048

SOLVENT

DMSO

NS

2

DS

8

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INSTRUM spect PROBHD 5 mm PABBO BB/

2.5

PULPROG

cosygpppqf


3.0


3.5


4.0


4.5


5.0


5.5


6.0


6.5


7.0


7.5


8.0


8.5


9.0


SWH 4629.629 Hz

FIDRES 2.260561 Hz

AQ 0.2211840 sec

RG 38.22

DW 108.000 usec

DE 6.50 usec

TE 303.0 K

D0 0.00000300 sec

D1 1.93200600 sec

D11 0.03000000 sec

D12 0.00002000 sec

D13 0.00000400 sec

D16 0.00020000 sec

IN0 0.00021600 sec


======== CHANNEL f1 ======== SFO1 500.1914551 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 128

SFO1 500.1915 MHz

FIDRES 36.168980 Hz

SW 9.256 ppm

FnMODE QF


F2 - Processing parameters SI 1024

SF 500.1890000 MHz

WDW QSINE

SSB 0

LB 0 Hz

GB 0

PC 1.40


F1 - Processing parameters SI 1024

MC2 QF

SF 500.1890000 MHz

WDW QSINE

SSB 0

9 8 7 6 5 4 3

ppm

LB 0 Hz

GB 0


ppm 6.6


SD08-DMSO-COSYGP


Current Data Parameters NAME 11THAO SD08 EXPNO 7 PROCNO 1 F2 Acquisition Parameters Date 20200421 3

Current Data Parameters NAME 11THAO SD08 EXPNO 7 PROCNO 1 F2 Acquisition Parameters Date 20200421 4

Current Data Parameters NAME 11THAO_SD08

EXPNO 7

PROCNO 1

F2 - Acquisition Parameters Date_ 20200421

Time 18.30

INSTRUM spect PROBHD 5 mm PABBO BB/

PULPROG cosygpppqf

TD 2048

SOLVENT DMSO

NS 2

DS 8

6.8

SWH

4629.629 Hz


7.0


7.2


7.4

FIDRES 2.260561 Hz

AQ 0.2211840 sec

RG 38.22

DW 108.000 usec

DE 6.50 usec

TE 303.0 K

D0 0.00000300 sec

D1 1.93200600 sec

D11 0.03000000 sec

D12 0.00002000 sec

D13 0.00000400 sec

D16 0.00020000 sec

IN0 0.00021600 sec


======== CHANNEL f1 ======== SFO1 500.1914551 MHz

NUC1 1H

P0 10.20 usec

P1 10.20 usec


7.6


7.8


8.0


8.2


8.4


8.4


8.2


8.0


7.8


7.6


7.4


7.2


7.0


6.8


6.6


ppm

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 128

SFO1 500.1915 MHz

FIDRES 36.168980 Hz

SW 9.256 ppm

FnMODE QF


F2 - Processing parameters SI 1024

SF 500.1890000 MHz

WDW QSINE

SSB 0

LB 0 Hz

GB 0

PC 1.40


F1 - Processing parameters SI 1024

MC2 QF

SF 500.1890000 MHz

WDW QSINE

SSB 0

LB 0 Hz

GB 0


PL-9


SD08-DMSO-HMBC


ppm


30


40


50


60


70


80


90


100


110


120


130


140


150


160


170


180

SD08-DMSO-HMBC


ppm 95


100


105


110


115


120


125


130


135


140


145


150


155


160


165


170



8 7 6 5 4 3

190

5 PHỔ HMBC PL 10 ppm 8 5 8 0 7 5 7 0 6 5 6 0 5 5 5 0 4 5 4 0 3 5 175 3 0 ppm SD08 DMSO HMBC ppm 5

5. PHỔ HMBC

PL-10

ppm


8.5


8.0


7.5


7.0


6.5


6.0


5.5


5.0


4.5


4.0


3.5

175

3 0 ppm SD08 DMSO HMBC ppm SD08 DMSO HSQC ppm 8 0 7 5 7 0 6 5 6 0 100 105 110 6 PHỔ HSQC 115 120 6

3.0 ppm


SD08-DMSO-HMBC


ppm

SD08-DMSO-HSQC


ppm


8.0 7.5


7.0


6.5


6.0


100


105 110 6 PHỔ HSQC 115 120 125 130 135 140 145 150 ppm 9 8 7 6 5 4 3 35 40 45 50 55 60 65 70 75 7

105


110


6. PHỔ HSQC

115


120


125


130


135


140


145


150


ppm


9 8 7


6 5 4 3


35


40 45 50 55 60 65 70 75 PL 11 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 ppm SD08 DMSO 8

40


45


50


55


60


65


70


75


PL-11

80


85


90


95


100


105


110


115


120


125


130


135


140


145


150

ppm


SD08 DMSO HSQC ppm 100 105 110 115 120 125 130 135 140 8 4 8 2 8 0 7 8 7 6 7 4 7 2 7 0 6 8 6 6 6 4 9

SD08-DMSO-HSQC

ppm

100

105

110

115

120

125

130

135

140

8.4 8.2 8.0 7.8 7.6 7.4 7.2 7.0 6.8

6.6 6.4 6.2

ppm

7. PHỔ NOESY


ppm


2.5


3.0


3.5


SD08-DMSO-NOESY



Current Data Parameters NAME 11THAO SD08 EXPNO 8 PROCNO 1 F2 Acquisition Parameters Date 20200421 10

Current Data Parameters NAME 11THAO SD08 EXPNO 8 PROCNO 1 F2 Acquisition Parameters Date 20200421 11

Current Data Parameters NAME 11THAO_SD08

EXPNO 8

PROCNO 1

F2 - Acquisition Parameters Date_ 20200421

Time 18.41

INSTRUM spect PROBHD 5 mm PABBO BB/

PULPROG noesygpphpp TD 2048

SOLVENT DMSO

NS 4

DS 32

SWH 4629.629 Hz

FIDRES 2.260561 Hz

AQ 0.2211840 sec

RG 38.22

DW 108.000 usec

DE 6.50 usec

TE 303.0 K

4.0


4.5


5.0


5.5


6.0


6.5


7.0


7.5


8.0


8.5


9.0

9


8 7 6 5 4 3


ppm

D0 0.00009501 sec

D1 1.98361599 sec

D8 0.30000001 sec

D11 0.03000000 sec

D12 0.00002000 sec

D16 0.00020000 sec

IN0 0.00021600 sec


======== CHANNEL f1 ======== SFO1 500.1914553 MHz

NUC1 1H

P1 10.20 usec

P2 20.40 usec

P17 2500.00 usec

PLW1 22.00000000 W

PLW10 2.54320002 W


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

GPZ1 40.00 %

P16 1000.00 usec

F1 - Acquisition parameters TD 256

SFO1 500.1915 MHz

FIDRES 36.168980 Hz

SW 9.256 ppm

FnMODE States-TPPI


F2 - Processing parameters SI 1024

SF 500.1890056 MHz

WDW QSINE

SSB 2

LB 0 Hz

GB 0

PC 1.00


F1 - Processing parameters SI 1024

MC2 States-TPPI

SF 500.1890046 MHz

WDW QSINE

SSB 2

LB 0 Hz

GB 0

SD08 DMSO NOESY ppm 6 6 6 8 7 0 7 2 7 4 7 6 7 8 8 0 8 2 8 4 8 4 8 2 8 0 7 8 7 6 7 4 7 2 7 0 6 8 6 6 12

SD08-DMSO-NOESY



ppm 6.6

6.8


7.0


7.2


7.4


7.6


7.8


8.0


8.2


8.4


8.4


8.2


8.0


7.8


7.6


7.4


7.2


7.0


6.8


6.6



ppm


Current Data Parameters NAME 11THAO_SD08

EXPNO 8 PROCNO 1 F2 Acquisition Parameters Date 20200421 Time 18 41 INSTRUM spect PROBHD 5 mm PABBO 13

EXPNO 8

PROCNO 1

F2 - Acquisition Parameters Date_ 20200421

Time 18.41

INSTRUM spect PROBHD 5 mm PABBO BB/

PULPROG noesygpphpp TD 2048

SOLVENT DMSO

NS 4

DS 32

SWH 4629.629 Hz

FIDRES 2.260561 Hz

AQ 0.2211840 sec

RG 38.22

DW 108.000 usec

DE 6.50 usec

TE 303.0 K

D0 0.00009501 sec

D1 1.98361599 sec

D8 0.30000001 sec

D11 0.03000000 sec

D12 0.00002000 sec

D16 0.00020000 sec

IN0 0.00021600 sec


======== CHANNEL f1 ======== SFO1 500.1914553 MHz

NUC1 1H

P1 10.20 usec

P2 20.40 usec

P17 2500.00 usec

PLW1 22.00000000 W

PLW10 2.54320002 W


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

GPZ1 40.00 %

P16 1000.00 usec


F1 - Acquisition parameters TD 256

SFO1 500.1915 MHz

FIDRES 36.168980 Hz

SW 9.256 ppm

FnMODE States-TPPI


F2 - Processing parameters SI 1024

SF 500.1890056 MHz

WDW QSINE

SSB 2

LB 0 Hz

GB 0

PC 1.00


F1 - Processing parameters SI 1024

MC2 States-TPPI

SF 500.1890046 MHz

WDW QSINE

SSB 2

LB 0 Hz

GB 0


ppm 2.8


2.9


3.0


3.1


SD08-DMSO-NOESY


Current Data Parameters NAME 11THAO SD08 EXPNO 8 PROCNO 1 F2 Acquisition Parameters Date 20200421 14

Current Data Parameters NAME 11THAO SD08 EXPNO 8 PROCNO 1 F2 Acquisition Parameters Date 20200421 15

Current Data Parameters NAME 11THAO_SD08

EXPNO 8

PROCNO 1

F2 - Acquisition Parameters Date_ 20200421

Time 18.41

INSTRUM spect PROBHD 5 mm PABBO BB/

PULPROG noesygpphpp TD 2048

SOLVENT DMSO

NS 4

DS 32

SWH 4629.629 Hz

FIDRES 2.260561 Hz

AQ 0.2211840 sec

RG 38.22

DW 108.000 usec

DE 6.50 usec

TE 303.0 K


3.2


3.3


3.4


3.5


3.6


3.7


3.8


3.9


4.0


4.1


8.5


8.0


7.5


7.0


6.5




ppm

D0 0.00009501 sec

D1 1.98361599 sec

D8 0.30000001 sec

D11 0.03000000 sec

D12 0.00002000 sec

D16 0.00020000 sec

IN0 0.00021600 sec


======== CHANNEL f1 ======== SFO1 500.1914553 MHz

NUC1 1H

P1 10.20 usec

P2 20.40 usec

P17 2500.00 usec

PLW1 22.00000000 W

PLW10 2.54320002 W


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

GPZ1 40.00 %

P16 1000.00 usec

F1 - Acquisition parameters TD 256

SFO1 500.1915 MHz

FIDRES 36.168980 Hz

SW 9.256 ppm

FnMODE States-TPPI


F2 - Processing parameters SI 1024

SF 500.1890056 MHz

WDW QSINE

SSB 2

LB 0 Hz

GB 0

PC 1.00


F1 - Processing parameters SI 1024

MC2 States-TPPI

SF 500.1890046 MHz

WDW QSINE

SSB 2

LB 0 Hz

GB 0

Phụ lục 3.2. Hợp chất SD2: Stedieltin B

CTPT: C17H11NO4 M = 293,0688

Chất kết tinh hình kim, màu trắng


MS

1H-NMR (500 MHz, CDCl3 + MeOD (9/1 v/v) và DMSO-d6)

13C-NMR (125 MHz, CDCl3 + MeOD (9/1 v/v) và DMSO-d6)

HMBC HSQC



1 PHỔ MS 2 PHỔ 1 H NMR 7 823 7 811 7 752 7 749 7 736 7 733 7 332 7 117 7 101 7 085 7 063 7 051 16

1. PHỔ MS


2 PHỔ 1 H NMR 7 823 7 811 7 752 7 749 7 736 7 733 7 332 7 117 7 101 7 085 7 063 7 051 6 964 6 961 17


2. PHỔ 1H-NMR


7.823

7.811

7.752

7.749

7.736

7.733

7.332

7.117

7.101

7.085

7.063

7.051

6.964

6.961

6.947

6.945

6.913

6.202

3.939

3.416

3.372

3.368

3.365

3.362

3.359

SD15.1-CDCl3+MeOD-1H



0 014 Current Data Parameters NAME 11THAO SD15 1 EXPNO 1 PROCNO 1 F2 Acquisition Parameters Date 21


-0.014

Current Data Parameters NAME 11THAO_SD15.1

EXPNO 1

PROCNO 1

F2 - Acquisition Parameters Date_ 20200426

Time 10.25

INSTRUM spect PROBHD 5 mm PABBO BB/ PULPROG zg30

TD 65536

SOLVENT CDCl3

NS 16

DS 2

SWH 10000.000 Hz

FIDRES 0.152588 Hz

AQ 3.2767999 sec

RG 198.57

DW 50.000 usec

DE 6 50 usec TE 303 0 K D1 1 00000000 sec TD0 1 CHANNEL f1 SFO1 500 1920889 MHz NUC1 1H P1 10 20 22

DE 6.50 usec

TE 303.0 K

D1 1.00000000 sec

TD0 1

======== CHANNEL f1 ======== SFO1 500.1920889 MHz NUC1 1H

P1 10.20 usec

PLW1 22.00000000 W

SI SF WDW

SSB


0

65536

500.1889759 MHz

EM

LB


0.30 Hz

GB

0


PC


1.00

F2 - Processing parameters


1.07

1.05

1.08

1.05

1.03

1.00

2.27

3.31


3.99

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



7.8

1.07

7.7

7.6

7.5

1.05



7.4

7.3

7.2

7.1

1.08

7.0

1.05


7.823

7.811


7.752

7.749

7.736

7.733


SD15.1-CDCl3+MeOD-1H

7.332


7.117

7.101

7.085

7.063

7.051


8.0

1.07

7.5

1.05


1.08

7.0

1.05

1.03

6.5

1.00



6.0

5.5

5.0

PL-16

2.27


7.823

7.811

7.752

7.749

7.736

7.733


7.332

7.117

7.101

7.085

7.063

7.051

6.964

6.961

6.947

6.945

SD15.1-CDCl3+MeOD-1H

6.913


6.202


1 03 4 5 6 964 6 961 6 947 6 945 3 31 3 939 4 0 3 5 3 416 6 9 1 00 6 913 ppm ppm 3 99 3 372 3 368 3 61

1.03


4.5

6.964

6 961 6 947 6 945 3 31 3 939 4 0 3 5 3 416 6 9 1 00 6 913 ppm ppm 3 99 3 372 3 368 3 365 3 362 3 359 64

6.961

6.947

6.945

3.313.939


4 0 3 5 3 416 6 9 1 00 6 913 ppm ppm 3 99 3 372 3 368 3 365 3 362 3 359 68

4.0

3.5

3.416

6.9

1.006.913

ppm

ppm

3.99

3.372

3.368

3.365

3.362

3.359

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