Triethylamine → N-[3-(3-Acetylthio-2-methylpropanoyl thio)-2-methyl-propanoyl]-N-cyclopentyl glycine-t-butyl ester

HRID 2164780ノート

反応式

HRID 2164780 の反応式
[C:1]([O:5][C:6](=[O:20])[CH2:7][N:8]([C:14](=[O:19])[CH:15]([CH3:18])[CH2:16][SH:17])[CH:9]1[CH2:13][CH2:12][CH2:11][CH2:10]1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:28]([S:31][CH2:32][CH:33]([CH3:37])[C:34](Cl)=[O:35])(=[O:30])[CH3:29]>C(Cl)Cl>[C:1]([O:5][C:6](=[O:20])[CH2:7][N:8]([C:14](=[O:19])[CH:15]([CH3:18])[CH2:16][S:17][C:34](=[O:35])[CH:33]([CH3:37])[CH2:32][S:31][C:28](=[O:30])[CH3:29])[CH:9]1[CH2:10][CH2:11][CH2:12][CH2:13]1)([CH3:2])([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 103458Ethanethioic acid, S-(3-chloro-2-methyl-3-oxopropyl) esterHCID 13469597N-(3-mercapto-2-methylpropanoyl)-N-cyclopentylglycine t-butyl ester

生成物 1

HCID 20037734N-[3-(3-Acetylthio-2-methylpropanoyl thio)-2-methyl-propanoyl]-N-cyclopentyl glycine-t-butyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of 3 g (0.01M) of N-(3-mercapto-2-methyl propanoyl)-N-cyclopentyl glycine-t-butyl ester, 1.2 g (0.012M) triethylamine in 100 ml methylene chloride was added a solution of 1.8 g (0.01M) of 3-acetylthio-2-methyl propanoyl chloride and stirring continued for 8 hours. It was then washed with water, dried over MgSO4 and evaporated to dryness leaving an oily residue which was purified by HPLC using ethyl acetate--hexane (1:3) as eluent.

後処理

  1. washIt was then washed with water
  2. dry with materialdried over MgSO4
  3. customevaporated to dryness
  4. customleaving an oily residue which
  5. customwas purified by HPLC

出典と根拠

ORDレコード
ord-e0def9c3adfc4501b7a0d5d5a38a1ede
出典データセット
uspto-grants-1985_03
特許番号
US04507316

反応ノート

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