反应详情

A mixture of 3.3g (0.01M) of 7-chloro-3,5-dihydro-2-(N-nitrosomethylamino)-5-phenyl-4H-1,5-benzodiazepin-4-one, 2g of acetylhydrazine, 5 ml of triethylamine and 50 ml of n-butanol was heated to reflux for 3 hrs. Half of the solvent was then removed by distillation and replaced by fresh n-butanol. Refluxing was continued for 3 days. The residue obtained after evaporation was chromotographed over 100 g of silical gel(Merck 70-230 mesh) using 10% (v/v) ethanol in methylene chloride for elution. Crystallization of the pure fraction from methylene chloride/ether yielded the above maned product, m.p. 298°-300°.

1. temperaturewas heated
2. temperatureto reflux for 3 hrs
3. customHalf of the solvent was then removed by distillation
4. temperatureRefluxing
5. customThe residue obtained
6. customafter evaporation
7. washfor elution
8. customCrystallization of the pure fraction from methylene chloride/ether
9. customyielded the above maned product, m.p. 298°-300°