반응식
[NH2:1][C:2]1[S:3][C:4]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Cl:15])=[O:8])=[CH:5][N:6]=1.[Cl:16][C:17]1[CH:34]=[CH:33][CH:32]=[CH:31][C:18]=1[C:19]([C:21]1SC(N=CN(C)C)=NC=1)=[O:20]>Cl>[NH2:1][C:2]1[S:3][C:4]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Cl:15])=[O:8])=[CH:5][N:6]=1.[Cl:16][C:17]1[CH:34]=[CH:33][CH:32]=[CH:31][C:18]=1[C:19](=[O:20])[CH3:21]참가 물질
5
반응 조건
- 온도
- 70 °C
실험 절차
(2-Amino-thiazol-5-yl)-(2-chloro-phenyl)-methanone The crude N′-[5-(2-chloro-benzoyl)-thiazol-2-yl]-N,N-dimethyl-formamidine was dissolved in 10% hydrochloric acid (150 mL) and heated at 70° C. for 4 hours. The precipitate was filtered, washed with ether, and then suspended in a 10% sodium carbonate solution (250 mL). The suspension was stirred for 1 hour and the precipitate was filtered, washed with ether, and dried in air to give (2-amino-thiazol-5-yl)-(2-chloro-phenyl)-methanone as a brown solid (8.5 g, 36 mmol, 55% from 1-(2-chloro-phenyl)-ethanone). ESI-MS m/z calc. 238.0. found 239.3 (M+1)+1; 1H NMR (DMSO) δ 7.25 (s, 1H), 7.42-7.55 (m, 4H), 8.35 (s, 2H).
후처리
- filtrationThe precipitate was filtered
- washwashed with ether
- filtrationthe precipitate was filtered
- washwashed with ether
- customdried in air
출처 및 근거
- ORD 기록
- ord-daa927d7ed8f4ad086825775a4ad1448
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08541453B2
연결된 노트
불러오는 중…