Methanol → HCID 15755327、化合物

HRID 2082235ノート

反応式

HRID 2082235 の反応式
[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]

参加物

6

反応物 4

HCID 887MethanolHCID 962Water2 回HCID 14798Sodium HydroxideHCID 130847N(alpha)-(N(alpha)-(N(alpha)-(tert-butyloxycarbonyl)glutaminyl)-N(1)-formyl-tryptophyl)phenylalanine benzyl ester

生成物 1

HCID 15755327HCID 15755327、化合物収率 80.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-9d796689b9a14390a5f49684e68e4e6d
出典データセット
uspto-grants-1993_02
特許番号
US05187156

反応ノート

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