反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[CH2:13][CH2:12][N:11]3[C:5]2=[C:6]([CH:25]=1)[C:7]([N:18]1[CH2:23][CH2:22][N:21]([CH3:24])[CH2:20][CH2:19]1)=[N:8][C:9]1[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=13>C(Cl)(Cl)Cl.[O-2].[O-2].[Mn+4]>[Cl:1][C:2]1[CH:3]=[C:4]2[CH:13]=[CH:12][N:11]3[C:5]2=[C:6]([CH:25]=1)[C:7]([N:18]1[CH2:23][CH2:22][N:21]([CH3:24])[CH2:20][CH2:19]1)=[N:8][C:9]1[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=13参加物
4
実験手順
To a solution of 4-chloro-6-(4-methyl-1-piperazinyl)-1,2,-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine (6 g, 17 mmoles), in chloroform (150 ml) was added manganese dioxide (10.5 g). The mixture was heated under reflux for 24 hours. The mixture was cooled, filtered and the solid was washed with dichloromethane (200 ml). The filtrate was then concentrated to dryness. The residue was purified by flash chromatography over a silica gel column (150 g), eluted with 2% methanol in dichloromethane (4 1) and 3% methanol in dichloromethane (2 1). Evaporation of the eluent gave 3.8 g (63%) of product. Recrystallization from toluene (40 ml) yielded the analytical sample, mp 170°-172° C.
後処理
- temperatureThe mixture was heated
- temperatureunder reflux for 24 hours
- temperatureThe mixture was cooled
- filtrationfiltered
- washthe solid was washed with dichloromethane (200 ml)
- concentrationThe filtrate was then concentrated to dryness
- customThe residue was purified by flash chromatography over a silica gel column (150 g)
- washeluted with 2% methanol in dichloromethane (4 1) and 3% methanol in dichloromethane (2 1)
- customEvaporation of the eluent
出典と根拠
- ORDレコード
- ord-0bb8514b145a49a0a50a32a54b848d34
- 出典データセット
- uspto-grants-1988_08
- 特許番号
- US04761412
関連ノート
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