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

HRID 370844

반응식

HRID 370844 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1d6fdac4744840cfb5dd1e2285f22cac
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528282

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