反应详情

300 ml of 25% aqueous ammonia solution and 100 ml of methanol were added to a solution of 18.5 g of 7-chloro-5-(2-pyridyl)-3H-1,4-benzodiazepine-2(1H)-thione in 800 ml of tetrahydrofuran. The mixture was stirred at room temperature for 17 h., with the solution which formed being concentrated to about 200 ml in a vacuum. The crystals were filtered off, washed with water and dried, stirred in 25 ml of dioxan at 100° C., cooled and filtered off. There were obtained 16.3 g of 2-amino-7-chloro-5-(2-pyridyl)-3H-1,4-benzodiazepine which was used without further purification for the next step. A sample recrystallized from dioxan melted at 213-215° C.

1. customformed
2. concentrationbeing concentrated to about 200 ml in a vacuum
3. filtrationThe crystals were filtered off
4. washwashed with water
5. customdried
6. stirringstirred in 25 ml of dioxan at 100° C.
7. temperaturecooled
8. filtrationfiltered off