反应详情

A mixture of ethanol (300 ml) and hexamethylenetetramine (20 g., 0.143 mol) was stirred, heated to reflux, and saturated with ammonia. 2-Chloroacetamidobenzophenone (18.1 g., 0.066 mol) was added in small increments over 3 to 4 hours while a steady stream of ammonia was bubbled into the reaction mixture. Refluxing was continued for 3 hours after complete addition of 2-chloroacetamidobenzophenone. The flow of ammonia was interrupted and the ethanol removed by distillation in vacuo. The residue obtained was taken up in chloroform (200 ml), and washed with water (100 ml) at 50° C. The chloroform layer was evaporated to dryness at 30° C. and the oily solid obtained was recrystallized from toluene (100 ml) to give 1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one (13.2 g., 86%), melting at 184°-186° C.

1. temperatureheated
2. temperatureto reflux
3. customwas bubbled into the reaction mixture
4. temperatureRefluxing
5. additionafter complete addition of 2-chloroacetamidobenzophenone
6. customthe ethanol removed by distillation in vacuo
7. customThe residue obtained
8. washwashed with water (100 ml) at 50° C
9. customThe chloroform layer was evaporated to dryness at 30° C.
10. customthe oily solid obtained
11. customwas recrystallized from toluene (100 ml)