反応式
[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]1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-7746469717dd40258fff531d5fb7e20e
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05622947
関連ノート
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