反应详情

300 ml of 25% aqueous ammonia solution were added to a solution of 16 g of 7-nitro-5-phenyl-3H-1,4-benzodiazepine-2(1H)-thione (J. B. Hester, A. D. Rudzik & B. V. Kamdar, J.Med.Chem., 1971, 14, 1078-1081) in 850 ml of tetrahydrofuran. The solution was stirred at room temperature for 20 h. and then concentrated to about 50 ml in a vacuum. The crystalline precipitate was filtered off and recrystallized from dioxan. There were obtained 8.0 g of 2-amino-7-nitro-5-phenyl-3H-1,4-benzodiazepine which was used in this form for the next step.

1. concentrationconcentrated to about 50 ml in a vacuum
2. filtrationThe crystalline precipitate was filtered off
3. customrecrystallized from dioxan