Diisopropylethylamine → N-Carbobenzoxy-O-Benzyl-L-Aspartyl-L-Prolyl-L-Arginine

HRID 249070

반응식

HRID 249070 반응식
Cl.[NH2:2][C@H:3]([C:11]([OH:13])=[O:12])[CH2:4][CH2:5][CH2:6][NH:7][C:8](=[NH:10])[NH2:9].O.ON1[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2N=N1.[CH:25](N(C(C)C)CC)(C)C.[N+](C1C=CC(O[C:44](=[O:75])[C@@H:45]2[CH2:49][CH2:48][CH2:47][N:46]2[C:50](=[O:74])[C@H:51]([CH:63](CC2C=CC=CC=2)[C:64](=[O:66])[OH:65])[NH:52][C:53]([O:55][CH2:56][C:57]2[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=2)=[O:54])=CC=1)([O-])=O>O.CN(C)C=O>[C:53]([NH:52][C@H:51]([C:50]([N:46]1[CH2:47][CH2:48][CH2:49][C@H:45]1[C:44]([NH:2][C@H:3]([C:11]([OH:13])=[O:12])[CH2:4][CH2:5][CH2:6][NH:7][C:8](=[NH:9])[NH2:10])=[O:75])=[O:74])[CH2:63][C:64](=[O:66])[O:65][CH2:25][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)([O:55][CH2:56][C:57]1[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=1)=[O:54]

참가 물질

7

반응물 4

HCID 81531Diisopropylethylamine2회HCID 27960291-Hydroxybenzotriazole hydrateHCID 53695211N-Carbobenzoxy-beta-Benzyl-L-Aspartyl-L-Proline p-Nitrophenyl EsterHCID 178479459HCID 178479459, 화합물

생성물 1

HCID 178512864N-Carbobenzoxy-O-Benzyl-L-Aspartyl-L-Prolyl-L-Arginine

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매2회

실험 절차

Arginine hydrochloride (2.3 Kg) and 1-hydroxybenzotriazole hydrate (1.5 Kg) are dissolved in a mixture of distilled water (5-6 L) and dimethylformamide (10-12 L). The pH of the solution is adjusted to 7.0-7.5 by addition of diisopropylethylamine. N-carbobenzoxy-β-benzyl-L-aspartyl-L-proline p-nitrophenyl ester (5.8 Kg) is dissolved in dimethylformamide (5-10 L) and added, maintaining the pH of solution at 7.0-7.5 with diisopropylethylamine. The solution is stirred at 20°-30° C. until the pH remains constant. The solids are collected on a filter, rinsed with a mixture of dimethylformamide (20-25 L) and distilled water (20-25 L), followed by distilled water 20-30 L). The product is dissolved in acetic acid (12-15 L) and the solution is diluted with distilled water (50-60 L). The pH is adjusted to 4.0-4.5 by addition of dilute sodium hydroxide. The solids are collected on a filter and washed with distilled water followed by acetone and then dried below 60° C.

후처리

  1. additionadded
  2. customThe solids are collected on a filter
  3. washrinsed with a mixture of dimethylformamide (20-25 L)
  4. distillationdistilled water (20-25 L)
  5. distillationby distilled water 20-30 L)
  6. dissolutionThe product is dissolved in acetic acid (12-15 L)
  7. additionthe solution is diluted with distilled water (50-60 L)
  8. additionThe pH is adjusted to 4.0-4.5 by addition of dilute sodium hydroxide
  9. customThe solids are collected on
  10. filtrationa filter
  11. washwashed with distilled water
  12. customdried below 60° C.

출처 및 근거

ORD 기록
ord-639fba745f4e48c6bd810930af7a4381
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05212287

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