N-[1,1-dimethoxycarbonyl-4-oxo-4-(2-thienyl)butyl]-L-alanyl-L-proline t-butyl ester → N-[1-methoxycarbonyl-4-oxo-4-(2-thienyl)butyl]-L-alanyl-L-proline t-butyl ester

HRID 370846

反応式

HRID 370846 の反応式
[C:1]([O:5][C:6](=[O:35])[C@@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1[C:12](=[O:34])[C@H:13]([CH3:33])[NH:14][C:15](C(OC)=O)([C:25]([O:27][CH3:28])=[O:26])[CH2:16][CH2:17][C:18](=[O:24])[C:19]1[S:20][CH:21]=[CH:22][CH:23]=1)([CH3:4])([CH3:3])[CH3:2]>CO.O>[C:1]([O:5][C:6](=[O:35])[C@@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1[C:12](=[O:34])[C@H:13]([CH3:33])[NH:14][CH:15]([C:25]([O:27][CH3:28])=[O:26])[CH2:16][CH2:17][C:18](=[O:24])[C:19]1[S:20][CH:21]=[CH:22][CH:23]=1)([CH3:3])([CH3:2])[CH3:4]

参加物

4

反応物 1

HCID 70443263N-[1,1-dimethoxycarbonyl-4-oxo-4-(2-thienyl)butyl]-L-alanyl-L-proline t-butyl ester

生成物 1

HCID 70484536N-[1-methoxycarbonyl-4-oxo-4-(2-thienyl)butyl]-L-alanyl-L-proline t-butyl ester

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Aqueous N-sodium hydroxide solution (6.2 ml.) was added to a solution of N-[1,1-dimethoxycarbonyl-4-oxo-4-(2-thienyl)butyl]-L-alanyl-L-proline t-butyl ester (Example 31; 3.0 g.) in a mixture of methanol (3 ml.) and water (1.5 ml.) and the mixture was stirred at laboratory temperature for 16 hours and then evaporated to dryness under reduced pressure. The mixture was partitioned between water and ethyl acetate and the aqueous layer was separated, acidified to pH 5 with aqueous N-hydrochloric acid and extracted with dichloromethane. The extract was dried over magnesium sulphate and evaporated to dryness. There was thus obtained as residual oil N-[1-methoxycarbonyl-4-oxo-4-(2-thienyl)butyl]-L-alanyl-L-proline t-butyl ester.

後処理

  1. customevaporated to dryness under reduced pressure
  2. customThe mixture was partitioned between water and ethyl acetate
  3. customthe aqueous layer was separated
  4. extractionextracted with dichloromethane
  5. dry with materialThe extract was dried over magnesium sulphate
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-0d72e48250804d1f9118cef71c806eb6
出典データセット
uspto-grants-1985_07
特許番号
US04528282

関連ノート

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