반응식
[H-].[Na+].[CH2:3]([C:5]1[NH:6][CH:7]=[CH:8][N:9]=1)[CH3:4].[CH2:10]([O:12][C:13]([C:15]1[C:16]([CH2:39]Cl)=[N:17][C:18]2[C:23]([C:24]=1[C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=1)=[CH:22][C:21]([O:35][CH3:36])=[C:20]([O:37][CH3:38])[CH:19]=2)=[O:14])[CH3:11].O>CN(C)C=O>[CH2:10]([O:12][C:13]([C:15]1[C:16]([CH2:39][N:6]2[CH:7]=[CH:8][N:9]=[C:5]2[CH2:3][CH3:4])=[N:17][C:18]2[C:23]([C:24]=1[C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=1)=[CH:22][C:21]([O:35][CH3:36])=[C:20]([O:37][CH3:38])[CH:19]=2)=[O:14])[CH3:11]참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
Oily sodium hydride (60%, 0.323 g) was added to a solution of 2-ethylimidazole (0.776 g) in N,N-dimethylformamide (30 ml), followed by stirring at room temperature for 15 minutes. Then 2-chloromethyl-6,7-dimethoxy-4-(3,4-dimethoxyphenyl)quinoline-3-carboxylic acid ethyl ester (3.0 g) was added. After stirring at 80° C. for 1 hour, the reaction mixture was poured over water, and the separating crystal was collected by filtration, which was then recrystallized from ethanol to yield 6,7-dimethoxy-4-(3,4-dimethoxyphenyl)-2-(2-ethylimidazol-1-ylmethyl)quinoline-3-carboxylic acid ethyl ester (2.5 g, 74%) as a colorless prismatic crystal having a melting point of 163 to 164° C.
후처리
- stirringAfter stirring at 80° C. for 1 hour
- filtrationthe separating crystal was collected by filtration, which
- customwas then recrystallized from ethanol
출처 및 근거
- ORD 기록
- ord-f48f01cfd3164e4b847fada34eb206b6
- 출처 데이터셋
- uspto-grants-1999_08
- 특허 번호
- US05932592
연결된 노트
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