반응식
[BH4-].[Li+].C([O:5][C:6]([CH2:8][O:9][CH:10]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[N:14]([C:22](=[O:39])[C:23]2[CH:28]=[CH:27][C:26]([NH:29][C:30](=[O:38])[C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=3[CH3:37])=[CH:25][CH:24]=2)[CH2:13][CH2:12][CH2:11]1)=O)C.Cl>O1CCCC1>[OH:5][CH2:6][CH2:8][O:9][CH:10]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[N:14]([C:22](=[O:39])[C:23]2[CH:28]=[CH:27][C:26]([NH:29][C:30](=[O:38])[C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=3[CH3:37])=[CH:25][CH:24]=2)[CH2:13][CH2:12][CH2:11]1참가 물질
반응물 3
생성물 1
시약·촉매·용매 1
실험 절차
0.28 g of lithium borohydride was added to a solution of 2.2 g of 5-ethoxycarbonylmethoxy-7-chloro-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzo-azepine dissolved in 50 ml of tetrahydrofuran, at room temperature with stirring. The mixture was refluxed for 30 minutes. The reaction mixture was poured into a diluted hydrochloric acid. The mixture was subjected to extraction with dichloromethane. The extract was dried over magnesium sulfate and subjected to vacuum distillation to remove the solvent. The residue was purified by silica gel column chromatography (elutant: dichloromethane/methanol=100/1→50/1) and then recrystallized from dichloromethane-diethyl ether to obtain 1.6 g of 5-(2-hydroxyethoxy)-7-chloro-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine.
후처리
- temperatureThe mixture was refluxed for 30 minutes
- extractionThe mixture was subjected to extraction with dichloromethane
- dry with materialThe extract was dried over magnesium sulfate
- distillationsubjected to vacuum distillation
- customto remove the solvent
- customThe residue was purified by silica gel column chromatography (elutant: dichloromethane/methanol=100/1→50/1)
- customrecrystallized from dichloromethane-diethyl ether
출처 및 근거
- ORD 기록
- ord-7746469717dd40258fff531d5fb7e20e
- 출처 데이터셋
- uspto-grants-1997_04
- 특허 번호
- US05622947
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