Methanol → HCID 15755327, 화합물

HRID 2082235노트

반응식

HRID 2082235 반응식
[NH:1]([C:45]([O:47][C:48]([CH3:51])([CH3:50])[CH3:49])=[O:46])[C@H:2]([C:8]([NH:10][C@@H:11]([C:24]([NH:26][C@H:27]([C:35]([O:37]CC1C=CC=CC=1)=[O:36])[CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=[O:25])[CH2:12][C:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[N:15](C=O)[CH:14]=1)=[O:9])[CH2:3][CH2:4][C:5](=[O:7])[NH2:6].[OH-].[Na+].CO.O>C1COCC1>[NH:1]([C:45]([O:47][C:48]([CH3:51])([CH3:50])[CH3:49])=[O:46])[C@H:2]([C:8]([NH:10][C@@H:11]([C:24]([NH:26][C@H:27]([C:35]([OH:37])=[O:36])[CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=[O:25])[CH2:12][C:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[NH:15][CH:14]=1)=[O:9])[CH2:3][CH2:4][C:5](=[O:7])[NH2:6]

참가 물질

6

반응물 4

HCID 887MethanolHCID 962Water2회HCID 14798Sodium HydroxideHCID 130847N(alpha)-(N(alpha)-(N(alpha)-(tert-butyloxycarbonyl)glutaminyl)-N(1)-formyl-tryptophyl)phenylalanine benzyl ester

생성물 1

HCID 15755327HCID 15755327, 화합물수율 80.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of Boc-Gln-D-Trp(CHO)-Phe-OBzl (1.2 g) and 1N sodium hydroxide (3.6 ml) in a mixture of THF (30 ml), methanol (10 ml) and water (5 ml) was stirred for 1.5 hours. After adding water (10 ml), the organic solvent was evaporated. The resulting aqueous solution was washed with diethyl ether, acidified with 10% citric acid solution and allowed to stand in a refrigerator overnight. The precipitates were filtered, washed with water and recrystallized with a mixture of ethanol and water to give Boc-Gln-D-Trp-Phe-OH (0.80 g).

후처리

  1. customthe organic solvent was evaporated
  2. washThe resulting aqueous solution was washed with diethyl ether
  3. customto stand in a refrigerator overnight
  4. filtrationThe precipitates were filtered
  5. washwashed with water
  6. customrecrystallized with a mixture of ethanol and water

출처 및 근거

ORD 기록
ord-9d796689b9a14390a5f49684e68e4e6d
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05187156

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