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4-Methylmorpholine → N-t-butoxycarbonyl-L-tyrosylglycyl-L-alanine benzyl ester

HRID 436955
ノート
印刷プレビュー

反応式

HRID 436955 の反応式
ClC1C=C(Cl)C(Cl)=CC=1O[C:11](=[O:29])[C@H:12]([CH2:21][C:22]1[CH:27]=[CH:26][C:25]([OH:28])=[CH:24][CH:23]=1)[NH:13][C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15].Cl.[CH2:31]([O:38][C:39](=[O:47])[C@H:40]([CH3:46])[NH:41][C:42](=[O:45])[CH2:43][NH2:44])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.CN1CCOCC1>C(Cl)Cl>[CH2:31]([O:38][C:39](=[O:47])[C@H:40]([CH3:46])[NH:41][C:42](=[O:45])[CH2:43][NH:44][C:11](=[O:29])[C@H:12]([CH2:21][C:22]1[CH:23]=[CH:24][C:25]([OH:28])=[CH:26][CH:27]=1)[NH:13][C:14]([O:16][C:17]([CH3:18])([CH3:19])[CH3:20])=[O:15])[C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 79724-MethylmorpholineHCID 13273165(2,4,5-trichlorophenyl) (2S)-3-(4-hydroxyphenyl)-2-[(2-methylpropan-2-yl)oxycarbonylamino]propanoateHCID 53328828Benzyl glycyl-L-alaninate hydrochloride

生成物 1

HCID 53750798N-t-butoxycarbonyl-L-tyrosylglycyl-L-alanine benzyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 17.6 parts N-t-butoxycarbonyl-L-tyrosine 2,4,5-trichlorophenyl ester, 9.0 parts glycyl-L-alanine benzyl ester hydrochloride and 1.2 parts N-methylmorpholine in 200 parts methylene chloride is stirred for 16 hours at room temperature. Removal of the solvent under reduced pressure affords a crude product which is purified by low pressure column chromatography to give N-t-butoxycarbonyl-L-tyrosylglycyl-L-alanine benzyl ester. The purified material is dissolved in 400 parts methanol. Then, 0.4 part palladium black metal catalyst is added and the mixture shaken with hydrogen at atmospheric pressure and room temperature for about 5 hours. The catalyst is removed by filtration, and the solvent is removed by evaporation under reduced pressure. The resulting material is purified by low-pressure chromatography to give N-t-butoxycarbonyl-L-tyrosylglycyl-L-alanine. This compound is represented by the following formula

後処理

  1. customRemoval of the solvent under reduced pressure
  2. customaffords a crude product which
  3. customis purified by low pressure column chromatography

出典と根拠

ORDレコード
ord-7dd09a1cefae4b53a49903cf89014486
出典データセット
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04028319

反応ノート

読み込み中…

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