反応式
[Br:1][C:2]1[CH:3]=[C:4]2[CH2:13][CH2:12][N:11]3[C:5]2=[C:6]([CH:26]=1)[C:7]([N:19]1[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]1)=[N:8][C:9]1[CH:17]=[C:16]([CH3:18])[CH:15]=[CH:14][C:10]=13>C(Cl)(Cl)Cl.[O-2].[O-2].[Mn+4]>[Br:1][C:2]1[CH:3]=[C:4]2[CH:13]=[CH:12][N:11]3[C:5]2=[C:6]([CH:26]=1)[C:7]([N:19]1[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]1)=[N:8][C:9]1[CH:17]=[C:16]([CH3:18])[CH:15]=[CH:14][C:10]=13参加物
4
実験手順
To a solution of 4-bromo-6-(4-methyl-1-piperazinyl)-9-methyl-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine (5.7 g, 13.8 mmoles) in chloroform (540 ml) was added manganese dioxide (25 gm), and the mixture was heated under reflux for 4 days. The mixture was filtered, and the filter cake washed with dichloromethane. The filtrate was concentrated under vacuum. The residue was purified on a silica gel column, eluted with 2% methanol/dichloromethane. The fractions (75-100 ml each) containing pure product were pooled and concentrated. Recrystallization from a small volume of 2-propanol yielded 2.41 g (42%) of product, mp 153°-155° C.
後処理
- temperaturethe mixture was heated
- temperatureunder reflux for 4 days
- filtrationThe mixture was filtered
- washthe filter cake washed with dichloromethane
- concentrationThe filtrate was concentrated under vacuum
- customThe residue was purified on a silica gel column
- washeluted with 2% methanol/dichloromethane
- additionThe fractions (75-100 ml each) containing pure product
- concentrationconcentrated
- customRecrystallization from a small volume of 2-propanol
出典と根拠
- ORDレコード
- ord-8c5a3f95d4184a32bed230d25ba2ea11
- 出典データセット
- uspto-grants-1987_05
- 特許番号
- US04663453
関連ノート
読み込み中…