Luận văn Khảo sát thành phần hóa học của hoa cây Sơn Cúc Hai Hoa wedelia biflora(l.) dc., họcúc (asteraceae)

PHỤ LỤC WEDE.FE1−CDCl3−1H 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 ppm 1 . 5 7 3 1 . 5 8 2 1 . 5 9 6 1 . 6 1 9 1 . 6 4 6 1 . 6 5 7 1 . 6 6 0 1 . 6 7 0 1 . 6 8 2 1 . 6 8 8 1 . 7 0 0 1 . 7 0 8 1 . 7 1 5 1 . 7 2 7 1 . 7 3 4 1 . 7 4 4 1 . 7 5 6 1 . 7 6 3 1 . 7 6 9 1 . 7 7 6 1 . 8 1 5 1 . 8 3 5 1 . 8 5 5 1 . 8 6 2 1 . 8 6 8 1 . 9 5 2 1 . 9 5 6 1 . 9 6 7 1 . 9 8 0 1 . 9 8 6 1 . 9 9 8 2 . 0 0 4 2 . 0 1 1 2 . 0 1 8 2 . 0 3 2 2 . 0 3 7 2 . 0 4 9 2 . 0 6 8 2 . 2 0 9 2 . 2 3 1 2 . 2 5 3 2 . 2 5 7 2 . 2 7 4 2 . 2 7 8 2 . 2 8 4 2 . 2 8 8 2 . 3 0 0 2 . 3 0 4 2 . 3 1 0 2 . 3 1 4 3 . 4 8 6 3 . 4 9 9 3 . 5 1 1 3 . 5 2 1 3 . 5 3 0 3 . 5 4 3 0 . 7 3 3 3 . 2 5 3 7 . 3 9 7 3 . 9 7 1 3 . 9 7 5 6 . 4 5 9 2 . 8 2 5 3 . 7 2 2 2 . 6 5 7 1 3 . 1 1 1 3 . 5 2 6 2 . 2 8 6 3 . 1 1 0 3 . 4 4 3 2 . 0 8 7 1 . 3 4 3 0 . 8 2 8 1 . 0 7 0 1 . 0 0 0 PC 1.00 GB 0 LB 0.30 Hz SSB 0 WDW EM SF 500.1300119 MHz SI 32768 F2 − Processing parameters SFO1 500.1335009 MHz PL1 −3.00 dB P1 5.85 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec D1 1.00000000 sec TE 301.2 K DE 6.00 usec DW 50.000 usec RG 64 AQ 3.2769001 sec FIDRES 0.152588 Hz SWH 10000.000 Hz DS 0 NS 16 SOLVENT CDCl3 TD 65536 PULPROG zg30 PROBHD 5 mm Multinucl INSTRUM av500 Time 9.59 Date_ 20081021 F2 − Acquisition Parameters PROCNO 1 EXPNO 1 NAME 111WEDE.FE1 Current Data Parameters 6 22 23 3 WEDE.FE1−CDCl3−C13CPD 200 180 160 140 120 100 80 60 40 20 0 ppm 2 1 . 0 8 5 2 1 . 1 0 5 2 1 . 2 3 0 2 3 . 1 1 5 2 4 . 3 2 3 2 4 . 3 8 6 2 5 . 4 1 2 2 6 . 1 6 0 2 8 . 2 6 2 2 8 . 9 2 0 2 9 . 2 1 6 3 1 . 7 0 7 3 1 . 8 9 6 3 1 . 9 4 2 3 3 . 9 9 7 3 6 . 1 6 9 3 6 . 5 4 4 3 7 . 2 9 6 3 9 . 7 2 2 3 9 . 8 1 6 4 0 . 4 8 3 4 2 . 2 5 3 4 2 . 3 4 9 4 5 . 8 9 2 5 0 . 1 8 5 5 0 . 2 1 2 5 1 . 2 6 2 5 6 . 0 1 1 5 6 . 1 1 3 5 6 . 8 1 0 5 6 . 9 0 5 7 1 . 8 2 9 7 6 . 7 6 6 7 7 . 0 2 0 7 7 . 2 7 4 1 2 1 . 7 1 8 1 2 9 . 3 2 8 1 3 8 . 3 1 6 1 4 0 . 7 9 6 PC 1.00 GB 0 LB 1.00 Hz SSB 0 WDW EM SF 125.7577873 MHz SI 32768 F2 − Processing parameters SFO2 500.1320005 MHz PL13 20.50 dB PL12 19.62 dB PL2 −1.00 dB PCPD2 80.00 usec NUC2 1H CPDPRG2 waltz16 ======== CHANNEL f2 ======== SFO1 125.7703643 MHz PL1 −5.00 dB P1 13.00 usec NUC1 13C ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec DELTA 1.89999998 sec d11 0.03000000 sec D1 2.00000000 sec TE 300.2 K DE 6.00 usec DW 15.300 usec RG 8192 AQ 1.0027661 sec FIDRES 0.498653 Hz SWH 32679.738 Hz DS 2 NS 512 SOLVENT CDCl3 TD 65536 PULPROG zgpg30 PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 16.24 Date_ 20090104 F2 − Acquisition Parameters PROCNO 1 EXPNO 2 NAME 111WEDE.FE1 Current Data Parameters 5 22 23 6 3 WEDE.FE2−CDCl3−1H 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 ppm 1 . 4 4 5 1 . 4 5 8 1 . 4 8 4 1 . 4 9 2 1 . 5 0 9 1 . 5 1 8 1 . 5 2 7 1 . 5 3 8 1 . 5 5 1 1 . 5 5 9 1 . 5 7 2 1 . 5 9 1 1 . 6 0 4 1 . 6 3 4 1 . 6 3 8 1 . 6 4 8 1 . 6 6 5 1 . 6 7 5 1 . 6 9 2 1 . 7 3 8 1 . 7 4 7 1 . 7 6 5 1 . 7 7 4 1 . 7 9 2 1 . 8 0 2 1 . 8 1 3 1 . 8 3 4 1 . 8 5 0 1 . 8 5 8 1 . 8 6 3 1 . 8 7 1 1 . 8 7 7 1 . 8 9 3 1 . 9 0 0 1 . 9 1 0 1 . 9 3 0 1 . 9 3 6 1 . 9 6 0 1 . 9 6 9 1 . 9 8 8 1 . 9 9 7 2 . 0 0 8 2 . 0 1 5 2 . 0 2 4 3 . 2 0 7 3 . 2 1 5 3 . 2 2 9 5 . 1 2 9 5 . 1 3 6 5 . 1 7 7 5 . 1 8 4 5 . 1 9 1 7 . 2 6 1 1 . 8 7 6 5 . 2 4 1 3 . 4 8 7 5 . 7 9 5 4 . 8 1 3 4 . 6 2 7 5 . 4 5 0 2 . 0 1 1 2 . 5 3 5 2 . 0 4 5 4 . 2 2 6 2 . 3 4 8 4 . 9 4 3 3 . 2 5 7 1 . 6 3 8 1 . 0 9 2 1 . 4 5 4 0 . 8 3 8 1 . 4 4 7 0 . 7 6 3 1 . 0 5 0 1 . 0 0 0 PC 1.00 GB 0 LB 0.30 Hz SSB 0 WDW EM SF 500.1300125 MHz SI 32768 F2 − Processing parameters SFO1 500.1335009 MHz PL1 −1.00 dB P1 7.80 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec D1 1.00000000 sec TE 300.1 K DE 6.00 usec DW 50.000 usec RG 35.9 AQ 3.2769001 sec FIDRES 0.152588 Hz SWH 10000.000 Hz DS 0 NS 16 SOLVENT CDCl3 TD 65536 PULPROG zg30 PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 10.05 Date_ 20081103 F2 − Acquisition Parameters PROCNO 1 EXPNO 1 NAME 111WEDE.FE2 Current Data Parameters 12 3 W E D E . F E 2− CD Cl 3− 1H 0. 7 0. 8 0. 9 1. 0 1. 1 1. 2 1. 3 1. 4 1. 5 1. 6 p p m 0.727 0.731 0.751 0.792 0.802 0.814 0.819 0.833 0.872 0.914 0.926 0.939 0.956 0.970 0.998 1.011 1.024 1.028 1.033 1.073 1.081 1.088 1.107 1.114 1.120 1.136 1.198 1.204 1.210 1.224 1.230 1.237 1.255 1.310 1.318 1.324 1.343 1.349 1.360 1.383 1.396 1.403 1.413 1.422 1.431 1.445 1.458 1.484 1.492 1.509 1.518 1.527 1.538 1.551 1.559 1.572 1.591 1.604 1.634 1.638 1.876 5.241 3.487 5.795 4.813 4.627 5.450 2.011 2.535 2.045 4.226 2.348 4.943 3.257 27 23 26 25 29 30 28 24 WEDE.FE2−CDCl3−C13CPD 180 160 140 120 100 80 60 40 20 0 ppm 1 6 . 8 4 1 1 8 . 4 0 7 2 3 . 5 6 1 2 3 . 7 1 4 2 6 . 0 1 1 2 6 . 1 9 3 2 6 . 9 7 9 2 7 . 2 7 1 2 8 . 1 2 2 2 8 . 4 1 6 3 1 . 1 0 1 3 2 . 5 1 4 3 2 . 6 9 8 3 3 . 3 5 0 3 4 . 7 7 2 3 6 . 9 8 7 3 7 . 1 7 7 3 8 . 6 3 1 3 8 . 8 0 3 3 9 . 8 3 5 4 1 . 7 6 1 4 6 . 8 7 0 4 7 . 2 8 0 4 7 . 6 7 8 5 5 . 2 2 7 7 6 . 7 6 9 7 7 . 0 2 3 7 7 . 2 7 7 7 9 . 0 5 9 1 2 1 . 7 6 4 1 4 5 . 2 1 9 PC 1.40 GB 0 LB 1.00 Hz SSB 0 WDW EM SF 125.7577873 MHz SI 32768 F2 − Processing parameters SFO2 500.1320005 MHz PL13 20.50 dB PL12 19.22 dB PL2 −1.00 dB PCPD2 80.00 usec NUC2 1H CPDPRG2 waltz16 ======== CHANNEL f2 ======== SFO1 125.7703643 MHz PL1 −5.00 dB P1 13.20 usec NUC1 13C ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec DELTA 1.89999998 sec d11 0.03000000 sec D1 2.00000000 sec TE 300.1 K DE 6.00 usec DW 15.300 usec RG 2048 AQ 1.0027661 sec FIDRES 0.498653 Hz SWH 32679.738 Hz DS 2 NS 256 SOLVENT CDCl3 TD 65536 PULPROG zgpg30 PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 10.19 Date_ 20081103 F2 − Acquisition Parameters PROCNO 1 EXPNO 2 NAME 111WEDE.FE2 Current Data Parameters Phuï luïc 4: Phoå13C -N M R cuûa hôïp chaát W E D E .FE 2 13 12 3 5 WEDE.FE2−CDCl3−C13CPD 2030405060708090100110120130140150160170180190 ppm 2030405060708090100110120130140150160170180190 ppm 2030405060708090100110120130140150160170180190 ppm DEPT90 DEPT135 C13CPD CH&CH3 CH2 &DEPT Phuï luïc 5: Phoå D E PT-N M R cuûa hôïp chaát W E D E .FE 2 13 12 3 5 ppm 1.01.52.02.53.03.54.04.55.05.5 ppm 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 WEDE.FE2−CDCl3−COSYGP GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300119 MHz MC2 QF SI 1024 F1 − Processing parameters PC 1.40 GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300122 MHz SI 1024 F2 − Processing parameters FnMODE QF SW 9.997 ppm FIDRES 19.531250 Hz SFO1 500.1323 MHz TD 256 ND0 1 F1 − Acquisition parameters P16 1000.00 usec GPZ2 10.00 % GPZ1 10.00 % GPY2 0.00 % GPY1 0.00 % GPX2 0.00 % GPX1 0.00 % GPNAM2 SINE.100 GPNAM1 SINE.100 ====== GRADIENT CHANNEL ===== SFO1 500.1322506 MHz PL1 −1.00 dB P1 7.80 usec P0 7.80 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 1.48689198 sec MCREST 0.00000000 sec IN0 0.00020000 sec D16 0.00015000 sec d13 0.00000400 sec D1 1.48689198 sec d0 0.00000300 sec TE 300.0 K DE 6.00 usec DW 100.000 usec RG 45.3 AQ 0.2049500 sec FIDRES 2.441406 Hz SWH 5000.000 Hz DS 8 NS 8 SOLVENT CDCl3 TD 2048 PULPROG cosygpqf PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 10.39 Date_ 20081103 F2 − Acquisition Parameters PROCNO 1 EXPNO 5 NAME 111WEDE.FE2 Current Data Parameters 12 3 12 3 ppm 0.81.01.21.41.61.82.0 ppm 0.7 0.8 0.9 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 2.0 WEDE.FE2−CDCl3−COSYGP GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300119 MHz MC2 QF SI 1024 F1 − Processing parameters PC 1.40 GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300122 MHz SI 1024 F2 − Processing parameters FnMODE QF SW 9.997 ppm FIDRES 19.531250 Hz SFO1 500.1323 MHz TD 256 ND0 1 F1 − Acquisition parameters P16 1000.00 usec GPZ2 10.00 % GPZ1 10.00 % GPY2 0.00 % GPY1 0.00 % GPX2 0.00 % GPX1 0.00 % GPNAM2 SINE.100 GPNAM1 SINE.100 ====== GRADIENT CHANNEL ===== SFO1 500.1322506 MHz PL1 −1.00 dB P1 7.80 usec P0 7.80 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 1.48689198 sec MCREST 0.00000000 sec IN0 0.00020000 sec D16 0.00015000 sec d13 0.00000400 sec D1 1.48689198 sec d0 0.00000300 sec TE 300.0 K DE 6.00 usec DW 100.000 usec RG 45.3 AQ 0.2049500 sec FIDRES 2.441406 Hz SWH 5000.000 Hz DS 8 NS 8 SOLVENT CDCl3 TD 2048 PULPROG cosygpqf PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 10.39 Date_ 20081103 F2 − Acquisition Parameters PROCNO 1 EXPNO 5 NAME 111WEDE.FE2 Current Data Parameters 27 23 26 25 29 30 28 24 27 23 26 25 2930 28 24 5769 2 5 7 6 9 2 111 11 1 Phuï luïc 6a: Phoå C O SY cuûa hôïp chaát W E D E .FE 2 p p m 0 . 51 . 01 . 52 . 02 . 53 . 03 . 54 . 04 . 55 . 05 . 5 p p m 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 W E D E . F E 2 − C D C l 3 − H M B C 1 2 3 5 3 1 2 1 3 p p m 0 . 81 . 01 . 21 . 41 . 61 . 82 . 0 p p m 8 0 8 5 9 0 9 5 1 0 0 1 0 5 1 1 0 1 1 5 1 2 0 1 2 5 1 3 0 1 3 5 1 4 0 1 4 5 W E D E . F E 2 − C D C l 3 − H M B C 3 1 2 1 3 2 4 2 8 2 9 3 0 2 5 2 6 2 7 2 7 6 9 2 3 1 1 P h u ï l u ï c 7 a : P h o å H M B C c u û a h ô ï p c h a á t W E D E . F E 2 p p m 0 . 70 . 80 . 91 . 01 . 11 . 21 . 31 . 41 . 51 . 61 . 71 . 8 p p m 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 W E D E . F E 2 − C D C l 3 − H M B C 2 4 2 8 2 9 3 0 2 5 2 6 2 32 7 7 6 2 9 6 2 0 2 1 8 1 4 9 5 2 6 1 1 3 0 2 2 1 9 P h u ï l u ï c 7 b : P h o å H M B C c u û a h ô ï p c h a á t W E D E . F E 2 Print Date: 14 Jun 2009 09:32:31 Scan 12 from e:\du lieu ft-ms\6-2009\wede fe3.xms 100 200 300 400 500 600 700 m/z 0% 25% 50% 75% 100% 109.0 56351 149.0 53277 177.1 90513 202.6 98484 403.1 452427 404.1 194641 420.8 272146 421.8 68108 658.6 181960 660.4 55998 Spectrum 1A 0.115 min, Scan: 12, 100.0:1000.0>, RIC: 3.477e+6BP: 403.1 (452427=100%), wede fe3.xms Spectrum from e:\du lieu ft-ms\6-2009\wede fe3.xms Scan No: 12, Time: 0.115 minutes No averaging. Not background corrected. Comment: 0.115 min. Scan: 12 100.0:1000.0> RIC: 3.477e+6 Pair Count: 680 MW: 0 Formula: None CAS No: None Acquired Range: 100.0 - 1000.0 m/z Method Description: APCI Scan 1 Channel Description: 100.0:1000.0> APCI;CID -;Det EDR;WI Q1 Cal Scan Information: cp = 0.0 mTorr Precursor Mass Range: 100.0 - 1000.0 m/z Phuï luïc 8: Phoå M S cuûa hôïp chaát W E D E .FE 3 WEDE.FE3−CDCl3−1H 7 6 5 4 3 2 1 0 ppm 1 . 5 0 1 1 . 5 1 0 1 . 5 2 1 1 . 5 3 4 1 . 5 7 0 1 . 5 7 9 1 . 5 9 3 1 . 6 0 7 1 . 6 2 2 1 . 6 3 3 1 . 6 4 4 1 . 6 6 4 1 . 6 7 1 1 . 6 8 6 1 . 6 9 5 1 . 7 1 9 1 . 8 1 7 1 . 8 2 3 1 . 8 3 8 1 . 8 4 5 1 . 8 5 1 1 . 8 6 0 1 . 8 7 3 1 . 8 8 2 1 . 8 8 8 1 . 9 1 7 1 . 9 2 2 1 . 9 3 7 1 . 9 4 3 1 . 9 9 4 2 . 0 0 0 2 . 0 0 6 2 . 0 2 2 2 . 0 2 8 2 . 0 3 3 2 . 0 4 2 2 . 1 3 3 2 . 1 4 2 2 . 1 6 1 2 . 1 7 0 2 . 2 6 2 2 . 2 7 8 2 . 2 9 3 2 . 3 0 8 4 . 1 8 1 4 . 1 9 1 4 . 2 0 9 4 . 2 1 9 4 . 2 3 2 4 . 2 4 2 4 . 4 8 6 4 . 4 9 8 4 . 5 0 8 4 . 5 1 8 5 . 1 8 4 5 . 1 9 1 5 . 1 9 8 6 . 2 4 1 1 2 . 9 4 1 3 . 0 8 5 4 . 2 0 6 4 . 8 0 6 3 . 3 0 7 3 5 . 8 7 5 1 2 . 2 9 2 1 . 7 2 4 0 . 9 5 0 2 . 0 8 6 1 . 0 0 0 1 . 0 1 8 1 . 0 0 6 PC 1.00 GB 0 LB 0.50 Hz SSB 0 WDW EM SF 500.1300124 MHz SI 32768 F2 − Processing parameters SFO1 500.1335009 MHz PL1 −1.00 dB P1 7.45 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec D1 1.00000000 sec TE 300.1 K DE 6.00 usec DW 50.000 usec RG 40.3 AQ 3.2769001 sec FIDRES 0.152588 Hz SWH 10000.000 Hz DS 0 NS 16 SOLVENT CDCl3 TD 65536 PULPROG zg30 PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 10.27 Date_ 20090101 F2 − Acquisition Parameters PROCNO 1 EXPNO 1 NAME 111WEDE.FE3 Current Data Parameters 12 3 16 2' 22 11 W E D E . F E 3− CD Cl 3− 1H 0. 8 0. 9 1. 0 1. 1 1. 2 1. 3 1. 4 1. 5 1. 6 1. 7 p p m 0.769 0.789 0.796 0.802 0.830 0.870 0.875 0.881 0.894 0.907 0.940 0.967 0.983 0.991 1.030 1.045 1.053 1.073 1.082 1.093 1.107 1.118 1.149 1.187 1.195 1.216 1.255 1.285 1.289 1.293 1.311 1.333 1.336 1.347 1.355 1.373 1.381 1.395 1.401 1.427 1.444 1.453 1.501 1.510 1.521 1.534 1.570 1.579 1.593 1.607 1.622 1.633 1.644 1.664 1.671 1.686 1.695 1.719 6.241 12.941 3.085 4.206 4.806 3.307 35.875 12.292 27 26 25 30 28 29 23 24 18 ' WEDE.FE3−CDCl3−C13CPD 200 180 160 140 120 100 80 60 40 20 0 ppm 2 4 . 5 3 4 2 5 . 1 9 5 2 8 . 1 2 2 2 9 . 2 0 1 2 9 . 2 7 6 2 9 . 3 7 4 2 9 . 4 8 4 2 9 . 6 0 3 2 9 . 6 5 4 2 9 . 6 9 4 3 0 . 5 6 9 3 1 . 9 4 3 3 2 . 8 9 4 3 4 . 8 7 9 3 5 . 2 5 1 3 5 . 9 9 9 3 6 . 7 9 1 3 7 . 3 6 2 3 7 . 7 8 9 3 8 . 4 9 3 3 8 . 5 8 7 3 9 . 5 3 3 3 9 . 5 9 7 4 0 . 1 2 9 4 4 . 0 9 4 4 6 . 9 6 0 5 5 . 3 3 1 6 0 . 7 8 8 6 7 . 0 4 0 7 6 . 7 6 8 7 7 . 0 2 2 7 7 . 2 7 6 8 0 . 5 5 0 1 2 5 . 0 7 1 1 3 8 . 0 7 1 1 7 3 . 6 9 0 PC 1.40 GB 0 LB 1.00 Hz SSB 0 WDW EM SF 125.7577863 MHz SI 32768 F2 − Processing parameters SFO2 500.1320005 MHz PL13 20.50 dB PL12 19.62 dB PL2 −1.00 dB PCPD2 80.00 usec NUC2 1H CPDPRG2 waltz16 ======== CHANNEL f2 ======== SFO1 125.7703643 MHz PL1 −5.00 dB P1 13.00 usec NUC1 13C ======== CHANNEL f1 ======== MCWRK 0.01500000 sec MCREST 0.00000000 sec DELTA 1.89999998 sec d11 0.03000000 sec D1 2.00000000 sec TE 300.9 K DE 6.00 usec DW 15.300 usec RG 4096 AQ 1.0027661 sec FIDRES 0.498653 Hz SWH 32679.738 Hz DS 2 NS 2048 SOLVENT CDCl3 TD 65536 PULPROG zgpg30 PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 17.59 Date_ 20090119 F2 − Acquisition Parameters PROCNO 1 EXPNO 2 NAME 111WEDE.FE3 Current Data Parameters 13 12 1' 3 16 18 5 9 14 WEDE.FE3−CDCl3−C13CPD 2030405060708090100110120130140150160170180190 ppm 2030405060708090100110120130140150160170180190 ppm 2030405060708090100110120130140150160170180190 ppm DEPT90 DEPT135 C13CPD CH&CH3 CH2 &DEPT Phuï luïc 11: Phoå D E PT cuûa hôïp chaát W E D E .FE 3 1' 13 12 3 16 18 5 9 14 ppm 1.01.52.02.53.03.54.04.55.05.5 ppm 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 WEDE.FE3−CDCl3−COSYGP GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300122 MHz MC2 QF SI 1024 F1 − Processing parameters PC 1.40 GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300125 MHz SI 1024 F2 − Processing parameters FnMODE QF SW 9.997 ppm FIDRES 19.531250 Hz SFO1 500.1323 MHz TD 256 ND0 1 F1 − Acquisition parameters P16 1000.00 usec GPZ2 10.00 % GPZ1 10.00 % GPY2 0.00 % GPY1 0.00 % GPX2 0.00 % GPX1 0.00 % GPNAM2 SINE.100 GPNAM1 SINE.100 ====== GRADIENT CHANNEL ===== SFO1 500.1322506 MHz PL1 −1.00 dB P1 7.45 usec P0 7.45 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 1.48689198 sec MCREST 0.00000000 sec IN0 0.00020000 sec D16 0.00015000 sec d13 0.00000400 sec D1 1.48689198 sec d0 0.00000300 sec TE 307.6 K DE 6.00 usec DW 100.000 usec RG 57 AQ 0.2049500 sec FIDRES 2.441406 Hz SWH 5000.000 Hz DS 8 NS 8 SOLVENT CDCl3 TD 2048 PULPROG cosygpqf PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 20.05 Date_ 20090119 F2 − Acquisition Parameters PROCNO 1 EXPNO 5 NAME 111WEDE.FE3 Current Data Parameters 12 3 16 2' 22 11 12 3 16 2' 22 11 ppm 0.81.01.21.41.61.82.02.2 ppm 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 WEDE.FE3−CDCl3−COSYGP GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300122 MHz MC2 QF SI 1024 F1 − Processing parameters PC 1.40 GB 0 LB 0.00 Hz SSB 0 WDW SINE SF 500.1300125 MHz SI 1024 F2 − Processing parameters FnMODE QF SW 9.997 ppm FIDRES 19.531250 Hz SFO1 500.1323 MHz TD 256 ND0 1 F1 − Acquisition parameters P16 1000.00 usec GPZ2 10.00 % GPZ1 10.00 % GPY2 0.00 % GPY1 0.00 % GPX2 0.00 % GPX1 0.00 % GPNAM2 SINE.100 GPNAM1 SINE.100 ====== GRADIENT CHANNEL ===== SFO1 500.1322506 MHz PL1 −1.00 dB P1 7.45 usec P0 7.45 usec NUC1 1H ======== CHANNEL f1 ======== MCWRK 1.48689198 sec MCREST 0.00000000 sec IN0 0.00020000 sec D16 0.00015000 sec d13 0.00000400 sec D1 1.48689198 sec d0 0.00000300 sec TE 307.6 K DE 6.00 usec DW 100.000 usec RG 57 AQ 0.2049500 sec FIDRES 2.441406 Hz SWH 5000.000 Hz DS 8 NS 8 SOLVENT CDCl3 TD 2048 PULPROG cosygpqf PROBHD 5 mm TXI 1H−13 INSTRUM av500 Time 20.05 Date_ 20090119 F2 − Acquisition Parameters PROCNO 1 EXPNO 5 NAME 111WEDE.FE3 Current Data Parameters 22 11 2' 27 26 25 30 2324 29 28 22 11 2' 27 26 25 30 2324 29 28 Phuï luïc 12a: Phoå C O SY cuûa hôïp chaát W E D E .FE 3 p p m 0 . 51 . 01 . 52 . 02 . 53 . 03 . 54 . 04 . 55 . 05 . 5 p p m 1 5 2 0 2 5 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 9 5 1 0 0 1 0 5 1 1 0 1 1 5 1 2 0 1 2 5 1 3 0 W E D E . F E 3 − C D C l 3 − H S Q C 1 4 9 5 1 8 1 6 3 1 2 1 2 3 1 6 2 ' 2 2 1 1 p p m 0 . 81 . 01 . 21 . 41 . 61 . 82 . 02 . 22 . 4 p p m 1 4 1 6 1 8 2 0 2 2 2 4 2 6 2 8 3 0 3 2 3 4 3 6 3 8 4 0 W E D E . F E 3 − C D C l 3 − H S Q C 2 ' 2 2 1 1 2 7 2 6 2 5 3 0 2 3 2 4 2 9 2 8 1 8 ' 2 5 2 9 6 3 0 2 8 1 7 ' 2 7 3 ' 2 3 4 ' 2 1 7 2 ' 1 0 4 1 8 P h u ï l u ï c 1 3 a : P h o å H S Q C c u û a h ô ï p c h a á t W E D E . F E 3 p p m 0 . 51 . 01 . 52 . 02 . 53 . 03 . 54 . 04 . 55 . 05 . 5 p p m 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 1 6 0 1 7 0 1 8 0 W E D E . F E 3 − C D C l 3 − H M B C 1 2 3 1 6 2 ' 2 2 1 1 1 4 9 5 1 8 1 6 3 1 2 1 3 1 ' p p m 0 . 81 . 01 . 21 . 41 . 61 . 82 . 02 . 22 . 4 p p m 5 5 6 0 6 5 7 0 7 5 8 0 8 5 9 0 9 5 1 0 0 1 0 5 1 1 0 1 1 5 1 2 0 1 2 5 1 3 0 1 3 5 1 4 0 1 4 5 1 5 0 1 5 5 1 6 0 1 6 5 1 7 0 1 7 5 W E D E . F E 3 − C D C l 3 − H M B C 2 ' 2 2 1 1 2 7 2 6 2 5 3 0 2 3 2 4 2 9 2 8 5 1 8 1 6 3 1 2 1 3 1 ' P h u ï l u ï c 1 4 a : P h o å H M B C c u û a h ô ï p c h a á t W E D E . F E 3 p p m 2 . 02 . 53 . 03 . 54 . 04 . 55 . 0 p p m 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5