Metoclopramide → HCID 14372582, 화합물

HRID 620260

반응식

HRID 620260 반응식
[NH2:1][C:2]1[C:17]([Cl:18])=[CH:16][C:5]([C:6]([NH:8][CH2:9][CH2:10][N:11]([CH2:14]C)[CH2:12]C)=[O:7])=[C:4]([O:19]C)[CH:3]=1.NC1C(Cl)=CC(C(NCCN(C)C)=O)=C(OC)C=1>>[NH2:1][C:2]1[C:17]([Cl:18])=[CH:16][C:5]([C:6]([NH:8][CH2:9][CH2:10][N:11]([CH3:14])[CH3:12])=[O:7])=[C:4]([OH:19])[CH:3]=1

참가 물질

3

반응물 2

HCID 4168MetoclopramideHCID 103785104-Amino-5-chloro-N-[2-(dimethylamino)ethyl]-2-methoxybenzamide

생성물 1

HCID 14372582HCID 14372582, 화합물수율 89%

실험 절차

The general procedure of Preparation 1A was repeated except that the 4-amino-5-chloro-N-[2-(diethylamino)ethyl]-2-methoxybenzamide utilized therein was replaced by 4-amino-5-chloro-N-[2-(dimethylamino)ethyl]-2-methoxybenzamide (prepared according to U.K. Pat. No. 1,793,771). The solvent (DMF) was removed in vacuo, and the residue treated with water and methylene chloride saturated with carbon dioxide, concentrated, and the crude product isolated in 89% yield by extraction with ethanol. A sample was chromatographed on a silica gel column usimg methylene chloride (97), methanol (3), ammonia (0.3) solvent system. The appropriate fractions were combined and concentrated in vacuo. The residue was crystallized from methanol to give the title compound as a colorless solid, mp. 163°-165°.

후처리

  1. customprepared
  2. customThe solvent (DMF) was removed in vacuo
  3. additionthe residue treated with water and methylene chloride saturated with carbon dioxide
  4. concentrationconcentrated
  5. customthe crude product isolated in 89% yield by extraction with ethanol
  6. customA sample was chromatographed on a silica gel column usimg methylene chloride (97), methanol (3), ammonia (0.3) solvent system
  7. concentrationconcentrated in vacuo
  8. customThe residue was crystallized from methanol

출처 및 근거

ORD 기록
ord-6127a8d94fc743ae828eae8a2d912673
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04820715

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