Hợp Chất Sd11: (6R,9S)-Roseosid


SD13-MeOD-HSQC


ppm 60


65


70


75


80


85


90


95


100



5.2 5.0


4.8


4.6


4.4


4.2


4.0


3.8


3.6


3.4


3.2

105


PL 81 ppm Phụ lục 3 11 Hợp chất SD11 6R 9S roseosid CTPT C 19 H 30 O 8 M 386 Bột vô 1

PL-81

ppm

Phụ lục 3.11. Hợp chất SD11: (6R,9S)-roseosid

CTPT: C19H30O8 M = 386

Bột vô định hình màu trắng


MS

1H-NMR (500 MHz, CD3OD)

13C-NMR (125 MHz, CD3OD)

HMBC HSQC


1. PHỔ MS


Display Report - Selected Window Selected Analysis


Analysis Name:


SD14.d Instrument: LC-MSD-Trap-SL


Print Date: 5/20/2020 12:03:24 PM

Method: Sample Name:

Quang_2020.m SD14

Operator:

2195410AE0000514

Acq. Date: 5/20/2020 12:01:44 PM

Analysis Info: Column Eclipse XDB-C18, 4.6 x150mm

MSD Trap Report v 4 A4 Opt2 Page 1 of 1 2 PHỔ 1 H NMR SD14 MeOD 1H 6 007 5 977 5 975 5 892 5 890 2


MSD Trap Report v 4 (A4-Opt2)

Page 1 of 1

2. PHỔ 1H-NMR


SD14-MeOD-1H


6 007 5 977 5 975 5 892 5 890 5 888 5 775 5 760 5 744 5 729 4 820 4 565 4 552 4 540 4 302 4 287 3 3


6 007 5 977 5 975 5 892 5 890 5 888 5 775 5 760 5 744 5 729 4 820 4 565 4 552 4 540 4 302 4 287 3 4

6.007

5.977

5.975

5.892

5.890

5.888

5.775

5.760

5.744

5.729

4.820

4.565

4.552

4.540

4.302

4.287

3.884

3.880

3.861

3.856

3.673

3.661

3.650

3.637

3.368

3.336

3.333

3.330

3.326

3.323

3.321

3.303

3.288

3.285

3.269

3.252

3.230

3.214

3.196

3.187

3.182

3.175

3.170

3.164

3.156

2.641

2.607

2.212

2.179

1.965

1.962

1.317

1.304

1.060

1.038

0.022

Current Data Parameters NAME 11THAO_SD14

EXPNO 10

PROCNO 1

F2 - Acquisition Parameters Date_ 20200326

Time 17.02

INSTRUM spect PROBHD 5 mm PABBO BB/ PULPROG zg30

TD 65536

SOLVENT MeOD

NS 16

DS 2

SWH 10000.000 Hz

FIDRES 0.152588 Hz

AQ 3.2767999 sec

RG 72.05

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 usec

PLW1 22.00000000 W

SI SF WDW

SSB


0

65536

500.1890000 MHz

EM

LB


0.30 Hz

GB

0


PC


1.00

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F2 - Processing parameters


1.02

1.00

1.00

1.13

1.11

1.20

1.15

2.18

1.13

1.12

1.07

1.05

3.14

3.16

6.29

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


6 008 6 007 5 977 5 975 5 892 5 890 5 888 5 775 5 760 5 744 5 729 4 820 4 565 4 552 4 540 4 302 4 9

6.008

6.007

5.977

5.975

5.892

5.890

5.888

5.775

5.760

5.744

5.729

4.820

4.565

4.552

4.540

4.302

4.287

3.884

3.880

3.861

3.856

3.673

3.661

3.650

3.637

SD14-MeOD-1H


1 02 1 00 1 00 1 13 1 11 1 20 1 15 6 2 6 1 6 0 5 9 5 8 5 7 5 6 5 5 5 4 5 3 5 2 5 1 5 0 4 9 4 8 4 7 10


1.02

1.00

1.00

1.13

1.11

1.20

1.15

6.2 6.1

6.0

5.9

5.8

5.7 5.6

5.5

5.4

5.3

5.2

5.1

5.0

4.9

4.8

4.7

4.6

4.5

4.4

4.3

4.2

4.1

4.0

3.9

3.8

3.7

ppm

3 326 3 323 3 321 3 303 3 293 3 288 3 285 3 279 3 269 3 252 3 230 3 214 3 196 3 187 3 182 3 175 3 25

3.326

3.323

3.321

3.303

3.293

3.288

3.285

3.279

3.269

3.252

3.230

3.214

3.196

3.187

3.182

3.175

3.170

3.164

3.156

3.151

2.641

2.607

2.212

2.179

1.965

1.962

1.317

1.304

1.060

1.038

SD14-MeOD-1H


2 18 1 13 1 12 1 07 1 05 3 14 3 16 6 29 3 5 3 4 3 3 3 2 3 1 3 0 2 9 2 8 2 7 2 6 2 5 2 4 2 3 2 2 2 1 26


2.18

1.13

1.12

1.07

1.05

3.14

3.16

6.29

3.5 3.4

3.3

3.2

3.1

3.0

2.9

2.8

2.7

2.6

2.5

2.4

2.3

2.2

2.1

2.0

1.9

1.8

1.7

1.6

1.5

1.4

1.3

1.2

1.1

ppm


3. PHỔ 13C-NMR


201.23

167.06

133.74

133.71

127.12

101.26

80.00

78.37

78.17

74.95

74.65

71.69

62.84

50.75

49.51

49.34

49.17

49.00

48.82

48.66

48.48

42.41

24.69

23.47

22.24

19.54

SD14-MeOD-C13CPD


220 200 180 160 140 120 100 80 60 40 20 0 ppm Current Data Parameters NAME 11THAO SD14 EXPNO 2 42


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



Current Data Parameters NAME 11THAO_SD14

EXPNO 2

PROCNO 1

F2 - Acquisition Parameters Date_ 20200328

Time 8.16

INSTRUM spect PROBHD 5 mm PABBO BB/

PULPROG zgpg30

TD 65536

SOLVENT MeOD

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 305.3 K

D1 2.00000000 sec

D11 0.03000000 sec

TD0 1

======== CHANNEL f1 ======== SFO1 125.7864591 MHz NUC1 13C

P1 10.00 usec

PLW1 88.00000000 W

======== CHANNEL f2 ======== SFO2 500.1910008 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

125.7724511 MHz

EM

LB


1.00 Hz

GB

0


PC


1.40

F2 - Processing parameters


133 74 130 133 71 SD14 MeOD C13CPD 125 120 115 127 12 110 105 100 95 90 PL 85 101 26 85 80 80 00 78 45

133.74

130

133.71


SD14-MeOD-C13CPD

125

120

115

127.12


110

105

100

95

90

PL-85

101.26


85

80

80.00

78.37

78.17


75

74.95

74.65


ppm

71.69


201.23


SD14 MeOD C13CPD 200 190 180 170 160 150 140 130 120 110 167 06 133 74 133 71 127 12 100 90 101 26 55

SD14-MeOD-C13CPD

200

190

180

170

160

150 140 130 120 110

167.06


133.74

133.71

127.12


100

90

101.26


80

80.00

78.37

78.17

74.95

70

74.65

71.69


60

62.84

50.75

49.51

49.34

50

49.17

49.00

48.82

40

48.66

48.48

30

42.41


24.69

23.47

20

22.24

ppm

19.54


SD14 MeOD HMBC ppm 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 SD14 MeOD 58

SD14-MeOD-HMBC


ppm 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 SD14 MeOD HMBC ppm 20 25 59

ppm 10

20


30


40


50


60


70


80


90


100


110


120


130


140


150


160


170


180


190


200

SD14-MeOD-HMBC


ppm


20


25


30


35


40


45


50


55


60


65


70


75


80


4. PHỔ HMBC

PL-86

6.0 5.5

5.0

4.5

4.0

3.5

3.0

2.5

2.0

1.5

1.0

ppm

6.0

5.8

5.6

5.4

5.2

5.0

4.8

4.6

4.4

4.2 ppm

PL 87 SD14 MeOD HMBC ppm 65 70 75 80 85 90 95 100 SD14 MeOD HMBC ppm 130 135 140 145 150 155 160 60

PL 87 SD14 MeOD HMBC ppm 65 70 75 80 85 90 95 100 SD14 MeOD HMBC ppm 130 135 140 145 150 155 160 61


PL-87

SD14-MeOD-HMBC


ppm


65


70


75


80


85


90


95


100

SD14-MeOD-HMBC


ppm


130


135


140


145


150


155


160


165


170

PL 88 SD14 MeOD HMBC ppm 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 SD14 62

PL 88 SD14 MeOD HMBC ppm 125 130 135 140 145 150 155 160 165 170 175 180 185 190 195 200 205 SD14 63


PL-88

SD14-MeOD-HMBC


ppm 125

130


135


140


145


150


155


160


165


170


175


180


185


190


195


200


205

SD14-MeOD-HMBC


ppm


20


25


30


35


40


45


50


55


60


65


70


75


80


85

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