ABS ABS ABS 2.63365 NM 3.82449 NM 3^55736 NM ABS 294.000 258.000 227.000 0414 ẳ:?slleu 93 SBU 2.0 0FF Page Basel irie • May 2007 600.00 PHỤ LỤC I NM Phổ uv chất HMt PHỤ LỤC • 250.00 Phổ MS chất HMj 350.00 450.00 550.00 ABS : -0.1997 -> 4.2457 NM : 202.00 -> 600.00 Basel ine Erase ụ ieu Re-scale Zoom Cursor ỉlTBn More Phụ lục I: Các phổ chất HMị Urite labels OTỊ the graph _ m/ z abund m/z abund m/ z abund 50.10 61.05 2245 72.15 477 Scan 79 (4.5896528 min): D-DIP100.D 51.10 9637 HM1 62.05 3919 73.05 3295 52.10 6968 63.05 9748 74.05 909 m/z 10617 64.05 1916 77.05 1525 53.10 File3485 C:\HPCHEM\1\DATA\D-DIP100.D 85.05 65.05 1005 78.05 558 54.10 Operator Phong Cau truc, Hoa hoc 86.05 11649 66.05 800 vien 79.05 3314 55.10 Acquired May 107 1:16 pm using AcqMethod DEFAULT 87.05 1874 67.05 1519 80.05 2607 56.10 Instrument 598 9B 91.05 6057 68.15 1487 81.05 11449 57.10 Sample Name MS 92.05 845 69.05 5215 82.05 1534 58.10 Misc Info HM1 93.05 1707 83.05 2847 59.10 vial 675 Number 70.05 CHC13 + CH30H 94.05 3801 71.05 3585 84.05 1414 60.10 95.05 Scan 79 (4 589 min): D-DIP100 D 96.05 HM1 97.05 98.05 abund m/z abund m/z abund m/z 657 119.05 1173 139.05 1174 99.15 531 121.05 785 143.10 304 101.05 360 123.05 468 149.00 574 105.05 m/ z 2233 124.05 345 152.00 322 107.05 2456 125.05 1098 154.00 43568 108.05 19952 126.05 3346 155.00 4122 109.05 2000 127.05 590 156.00 505 110.05 1311 129.05 1493 157.00 323 111.05 640 135.15 352 171.10 336 112.15 628 137.05 57376 184.00 320 113.05 549 138.05 5534 115.05 2590 334 1059 2337 482 687 339 854 895 4193 1049 >und CO na na na no na o t-< ws: co c/l X oỊ I co õ 03 õ> cõo h«l M ro Ổ c nã 63s: o h-* ro na o o o 1NO C lo a ro na (-* ro 50 na Q h ro o o (0 ( ■> 00 00 h-» H*cn h-* ro 3o B ro cn cQo n Ln tH T3 í cn CỨco tul-h •o -0 co hí ro ro h- 00 M too h-» r—* rt co co ro Di o to co co 00 N1II 07 o cn -o oo P3 M 07 (D o o o o *-» ho o o o£ U) 00 ct cn o o OIƠ^ CO (D X h£ a a a c £ N se CÁse 03 03 03 oo 1Ị X N N (D Ị N o 111 ri ririri ri na na 2; II ri M d H* o i 1 i jj Library Searched Quality ID s £ o £ D a D h3 o D 50 > n P3 *-» h-* M s: OlO so h-* 50 17 Ỉ3 p*5 C > H m n 2 n ri o o M H> cn r—* õ o h- II o o 07 co o oóõ o ac co 03 (D Ă> i ã o 11 (-* 00 m WDZ co H na na M H M s COOOG ắ z H* o m5nz tu rõ o s c D X g3 s ht tr r* o CO ct ri r 50 < X ri (D (D 1□ n hf ri n ri 50 X 21 (D cõ z o o sa > H o o rt D:\DATABASE\WILEY275.L Ũ3 c 91 CJ H* tu CO rt H* tu Benzoic acid, 3,4-dihydroxy3 rt o r—o to Hna co £ tu cid $$ o 3,4-Dỉhydroxybenzoic o 00 o o ro c to hj o co co o o Ơ7 ho H tu o droxybenzene vo 20 40 53 63 81 97 jlịLi 60 80 Jo 11 126 'lio jJ _ 140 0 01 92 83 57 66 89 :.58 00 3160 33 3 16 99 lốo —I—’—■—■——I—■—■—■—■—í I ' Current Data Parameters NAME KINH HM1 EXPNO PROCNO 1 ■ ' I 1 ' I ■ ' ■ I 1 KINH-HMl-DMS0-C13CPD F2 - Acquisition Parameters Date_ 20070516 Time 16 11.19 ^ 00 INSTRƯM av500 00 Cò PROBHD mm Multinucl 27 PULPROG zgpg30 TD 65536 SOLVENT CDC13 256 NS DS 32679.738Hz SWH 0.498653Hz FIDRES 1.0027661sec AQ RG 3649.1 15.300usec DW DE 6.00usec TE 303.1K DI 2.00000000sec dll 0.03000000sec DELTA 1.89999998sec MCREST 0.00000000sec MCWRK 0.01500000sec SI 32768 SF 125.7578513MHz WDW EM SSB LB 1.00Hz GB PC 1.00 T (T l LT > CT i o IT > rH ư~) f— vô LO 00 T-' I ======== CHANNEL fl ======== NUC1 13C P1 8.60 usec PL1 -1.00 dB SF01 125.7703643 MHz CHANNEL f2 ======== waltzl6 CPDPRG2 1H NUC2 88.0 usec PCPD2 -3.00 dB PL2 15.47 PL12 I 22.0 dB dB PL13 500.1320005 MHz SF02 I F2 - Processing parameters 130 165 12 160 ' I ' 120 155 ppm 150 145 140 135 irn ' * 11 ■'1' ■ ’1 ■ I I'" Tnr KINH-HM1-DMS0-C13CPD&DEPT DEPT90 DEPT135 ■ ■ ’ I I ■ ■ ■ 200 CH2 190 ỉ .,,,-,| 1-iỴ-ĩ-r-r 180 170 160 150 140 130 120 '"I '-"ị"' 110 100 "T" 90 80 ' ■ I" 70 60 T^prr H-ry^T- 50 40 "r" r T"r ”r 20 ■ I ppm r f —I— 155 KINH-HM1-DMSO-C13CPD&DEPT DU=C:/Bruker/XWIN-NMR, USER=VH_KINH, NAME=KINH_HM1, EXPN0=3, PR0CN0=1 DU=C:/Bruker/XWIN-NMR, USER=VH_KINH, NAME=KINH_HM1, EXPN0=4, DU=C:/Bruker/XWIN-NMR, USER=VH_KINH, NAME=KINH_HM1, EXPN0=2, Fl=215.OOOppm, F2=-5.OOOppm, MI=O.OOcm, MAXI=10000.OOcm, PC=1.400 PR0CN0=1 —I—’ PR0CN0=1 Fl=215.OOOppm, PC=1.400 145 Fl=240.OOOppm, F2=-5.OOOppm, F2=-5.OOOppm, MI=O.OOcm, MI=O.OOcm, MAXI=10000.OOcm, MAXI=10000.OOcm, PC=1.400 r r —I— DEPT90 140 r —I—’ 160 r —I—’ 145 r —I— 160 r 170 —I— 165 ■—I —’ 160 150 135 130 125 120 115 I ppm 145 DEPT135 r —I—’ 140 # 10 11 12 13 14 15 16 17 # F R E Q U E NC Y I NT E NS IT Y [ H z] [ P PM ] 837 03 11 67 76 0021 885 576 49 59 59 06 66 1 82 51 44 84 59 72 13 566 532 83 21 843 13 586 53 02 29 21 41 CH2 42 16 54 04 1 46 55 866 441 447 592 1 5.1 48 ' I 8'8 I 170 165 155 23 886 503 81 40 00 05 150 23 896 502 29 39 23 8 23 07 50 09 99 39 833 33 23 91 499 5 39 57 0 79 23 92 49 88 411 39 66 23 93 8 497 17 39 58 89 23 50 496 41 39 499 23 97 1 49 46 422 39 32 63 23 99 492 43 39 66 32 4013 49 04 45 8.9 99 AD D R ES S F R E Q U E NC Y IN T E NS IT Y [ H z] [P P M] 13 31 532 72 12 47 4046 I • T 1 46 ' 55.I9 91 r 11 41 51 42 42 447165 6 41 50150 1 5.1 52 155 170 4583 499 019 3 511 AD D R ES S FR E QU E N C Y I NT E NS IT Y AD D R ES S 140 135 130 125 120 115 135 130 125 120 115 C13CPD # ỉ ppm ppm [ H z] [ P PM ] 21 847 33 8.1 532 3 09 40 46 46 56 019 16 541 I 11 11 57 447 6 99 O 42 41 o 45 82 39 59 50 00 012 o * H21 00 121.844 o 121.684 s 116.540 2* H 115.115 TJ o w Hw M«] ơ) TI T TI T) z o co TJ T) sp i n a T tí M G 11 ns nnHH n} tí tí tí C! tí 11 is ìó tí M ocr00 M M F o t í 0 1 OM M 11 M 11 ỉ » Pí H 00 s: M O J M ỡ rõ n ữ 11 > TI H to ĩõ 11 « cõ > 11 o to liH 11 5 76 26 KINH-HM1-DMS0-C13CPD 167.276 149.959 TI TJ P3 z 0Jto X >< > c ft tí h ( o 0znH z ÍD > 03 144.846 M H* 0co M t b t c vQ g C tí -0 TJ M Í: c 0> co M 00 c M •0 cotot 00 M 00 ro0 t C c r c co N I c 0 Hơli M -0 co(0 00co X c ỈO £ R s a s aac s s oK N (Á N D tt 11N ( VO L 00 • • o I 1— Current 0 M n 0 00 M co tí M CO to o Ố 40.001 39.924 39.834 39.757 K < z t-3 c M ọog N ọ oT CU SF01 CPDPRG2 NUC2 PCPD2 PL2 PL12 PL13 SF02 125.7703643MHz _ ruaMMPT -F9- - -= LilrilNlNlliL waltzl6 1H 88.00usec -3.00dB 15.47dB 22.00dB 500.1320005MHz F2 - Processing parameters SI 32768 SF 125.7578513MHz WDW EM SSB LB 1.00Hz GB PC 1.00 KINH-HM1-DMSO-C13CPD&DEPT DEPT90 ■ ■ l I I 30 20 ppm DEPT135 1 .I J I r-, l-rrm I , - r , , ,-| Tị-, , I I ị I .T^rryrr T-,-,-r T- r, ị r I^r_1-I r, r, r, I .I r -| , I 200 CH2 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 -1—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I—I— ' I ' 170 165 I 160 155 145 140 135 130 r 125 120 ppm 40 30 20 ppm r —í— 150 DU=C:/Bruker/XÍỈIN-NMR, USER=VH_KINH, NAME=KINH_HM1, EXPN0=3, DU=C:/Bruker/XWIN-NMR, NAME=KINH_HM1, EXPN0=4, PR0CN0=1 DU=C:/Bruker/XWIN-NMR, USER=VH_KINH, USER=VH_KINH, NAME=KINH_HM1, EXPN0=2, PR0CN0=1 PR0CN0=1 Fl=215.OOOppm, F2=-5,OOOppm, MI=O.OOcm, MAXI=10000.OOcm, Fl=240.OOOppm, F2=-5.OOOppm, MI=O.OOcm, MAXI=10000.OOcm, PC=1.400 PC=1.400 —I— Fl=215.OOOppm, 130 F2=-5.OOOppm, MI=O.OOcm, MAXI=10000.OOcm, PC=1.400 KINH-HM1-DMSO-C13CPD&DEPT r r DEPT90 —I— 145 r —I— 140 —I— r 160 165 155 I 145 140 135 125 120 115 110 —' I ppm T DEPT135 # AD D R E SS 10 11 12 13 14 15 16 17 # 83 7 002 066 13 566 586 42 441 2 886 89165 6 39 07 39 17 39 29 39 8 39 50 39 71 39 92 401 AD D R ES S CH2 C13CPD # 160 1 33 8.1 40 46 42 42 4583 AD D R165 ES S —I— 145 FR E QU E N C Y IN T E NS IT Y [H z ] [P P M] 21 036 31 16 27 63 45 88 58 57 49 59 59 821 51 44 459 53 22 83 12 43 53 02 72 12 841 45 46 5 86 11 40 4476 59 11 11 88 03 0 00 81 '—I— 02 72 9 92 48 155 150 160 009 39 9 83 37 3 49 99 55 57 0 49 8 41 66 0.6 49 61 889 80 49 67 41 49 99 12 50 49 46 42 33 29 0.6 49 43 16 49 4 50 99 92 FR E QU E N C Y IN T E NS IT Y [ H z] [ P PM ] 532 72 21 847 46 55 91 16 541 51 447 6 41 11 11 52 50 499 019 39 51 1 F R E Q U155 E NC Y IN T E NS IT Y 150 —T—I 135 130 125 120 115 110 135 130 125 120 115 110 ppm —T—I 140 ppm ... 25 9 .20 26 0 .20 26 1 .20 26 7.30 26 8.30 26 9 .20 27 0 .20 27 1 .20 D-DIP1 12. D m/ z 591 9 52 356 20 6 374 24 3 581 700 367 623 579 698 22 5.15 22 6.15 22 7.15 22 8.15 22 9.15 23 0 .25 23 1 .25 23 2.15 23 3 .25 321 1 92 229 ... 24 2 .20 1079 24 3 .20 334 24 4 .20 1711 24 5 .20 498 24 6 .20 23 3 25 2 .20 171 25 3 .20 24 3 25 4 .20 376 25 5 .20 604 Scan 20 (0. 724 min) : RM2 m/z abund 327 .25 328 .25 329 .25 21 9.15 m/ z 27 2 .20 27 3 .20 27 4 .20 27 9 .20 ... 314 24 0 25 0 521 324 354 420 169.15 170.05 171.15 m/ z 21 3.15 21 4.15 21 7.15 21 8.15 21 9.05 22 0.15 22 2 .25 23 9.10 24 1.10 24 2.10 569 20 9 570 abund 26 3 197 22 1 25 4 25 7 24 6 21 2 23 5 22 29 4 92 181.15 1 82. 15