反应详情

Acetic acid (30 ml) was added to a slurry consisting of sodium cyanide (10 g), 1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]-benzodiazepine (19 g) and ethyl acetate (250 ml) dropwise at room temperature. The mixture was stirred for 18 hours and thereafter diluted with ethyl acetate to 1 liter and washed with 1N sodium hydroxide (2×500 ml), water (2×600 ml) and brine (2×600 ml) The solution was dried over anhydrous magnesium sulfate and concentrated to a solid. The solid was triturated with ether (2×150 ml). Recrystallization from hot toluene (450 ml) yielded 14.8 g of crystals, m.p. 185°-186.5° C.

1. washwashed with 1N sodium hydroxide (2×500 ml), water (2×600 ml) and brine (2×600 ml) The solution
2. dry with materialwas dried over anhydrous magnesium sulfate
3. concentrationconcentrated to a solid
4. customThe solid was triturated with ether (2×150 ml)
5. customRecrystallization from hot toluene (450 ml)