反应详情

0.245 g (0.005 mole) of sodium cyanide is added at 0°, with stirring, to the saturated solution of ammonia in 15 ml of isopropanol. After 5 minutes, a solution of 0.322 g (0.001 mole) of 6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine-1-carboxaldehyde in ca. 10 ml of isopropanol is added together with 0.87 g of manganese dioxide. After a further 10 minutes, another addition is made of 0.87 g (total 0.02 mole) of manganese dioxide, and the mixture stirred for 4 hours at 0°. After the addition of ca. 40 ml of methylene chloride, the reaction mixture is filtered and the filtrate concentrated by evaporation. Crystallisation of the residue from methanol/ethyl acetate/petroleum ether yields 6-phenyl-8-chloro-4H-s-triazolo[4,3-a][1,4]benzodiazepine-1-carboxamide, M.P. 285°-289°.

1. waitAfter a further 10 minutes
2. additionanother addition
3. filtrationthe reaction mixture is filtered
4. concentrationthe filtrate concentrated by evaporation
5. customCrystallisation of the residue from methanol/ethyl acetate/petroleum ether