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

HRID 370844

反応式

HRID 370844 の反応式
[C:1]([O:5][C:6](=[O:26])[C@@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1[C:12](=[O:25])[C@H:13]([CH3:24])[NH:14][CH:15]([C:20]([O:22][CH3:23])=[O:21])[C:16]([O:18][CH3:19])=[O:17])([CH3:4])([CH3:3])[CH3:2].Cl.CN(C)[CH2:30][CH2:31][C:32]([C:34]1[S:35][CH:36]=[CH:37][CH:38]=1)=[O:33].C(=O)([O-])[O-].[K+].[K+]>CO>[C:1]([O:5][C:6](=[O:26])[C@@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1[C:12](=[O:25])[C@H:13]([CH3:24])[NH:14][C:15]([C:16]([O:18][CH3:19])=[O:17])([C:20]([O:22][CH3:23])=[O:21])[CH2:30][CH2:31][C:32](=[O:33])[C:34]1[S:35][CH:36]=[CH:37][CH:38]=1)([CH3:2])([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 28768913-(Dimethylamino)-1-(thiophen-2-yl)propan-1-one hydrochlorideHCID 18598656N-(dimethoxycarbonylmethyl)-L-alanyl-L-proline t-butyl ester

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A-mixture of N-(dimethoxycarbonylmethyl)-L-alanyl-L-proline t-butyl ester (2.0 g.), 3-dimethylamino-1-(2-thienyl)propan-1-one hydrochloride (1.8 g.), potassium carbonate (2.0 g.) and methanol (15 ml.) was stirred at laboratory temperature for 16 hours and then evaporated to dryness under reduced pressure. The residue was stirred with dichloromethane, the mixture was filtered through a filter-aid and the filtrate was evaporated to dryness under reduced pressure. The residue was purified by chromatography on a silica gel column using a 19:1 v/v mixture of dichloromethane and ethyl acetate as eluant. There was thus obtained as an oil N-[1,1-dimethoxycarbonyl-4-oxo-4-(2-thienyl)butyl]-L-alanyl-L-proline t-butyl ester.

後処理

  1. customevaporated to dryness under reduced pressure
  2. filtrationthe mixture was filtered through
  3. filtrationa filter-aid
  4. customthe filtrate was evaporated to dryness under reduced pressure
  5. customThe residue was purified by chromatography on a silica gel column
  6. additiona 19:1 v/v mixture of dichloromethane and ethyl acetate as eluant

出典と根拠

ORDレコード
ord-1d6fdac4744840cfb5dd1e2285f22cac
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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