反应详情

6-Cyano-1,2,6,7-tetrahydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine (15 g) was added to 300 ml of a 1M solution of diisobutylaluminium hydride in dichloromethane at -78° C. The reaction mixture was stirred for 3 hours at low temperature and thereafter diluted to 1 liter with dichloromethane. The excess hydride was slowly decomposed with methanol (50 ml). The gelatinous solution was washed with 5% sodium hydroxide (500 ml) and brine (2×500 ml) and dried over anhydrous sodium sulfate. The solution was filtered and concentrated to a solid-oil mixture (15.2 g). Purification was effected by flash chromatography over silica gel (145 g, eluted with 3.5% methanol/dichloromethane) to afford 7.7 g of product. Recrystallization from hot ethanol (65 ml) yielded 6.2 g of crystals, m.p. 171.5°-172.5° C.

1. washThe gelatinous solution was washed with 5% sodium hydroxide (500 ml) and brine (2×500 ml)
2. dry with materialdried over anhydrous sodium sulfate
3. filtrationThe solution was filtered
4. concentrationconcentrated to a solid-oil mixture (15.2 g)
5. customPurification