反应详情

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.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 4 days
3. filtrationThe mixture was filtered
4. washthe filter cake washed with dichloromethane
5. concentrationThe filtrate was concentrated under vacuum
6. customThe residue was purified on a silica gel column
7. washeluted with 2% methanol/dichloromethane
8. additionThe fractions (75-100 ml each) containing pure product
9. concentrationconcentrated
10. customRecrystallization from a small volume of 2-propanol