反应详情

A suspension of 14.3g (0.05 mol) of 7-chloro-5-phenyl-1,2,3,5-tetrahydro-4H-1,5-benzodiazepin-2,4-dione in 1l of tetrahydrofuran and 200 ml of benzene was saturated with methylamine. A solution of 11.5 g (0.06 mol) of titanium tetrachloride in 200 ml of benzene was added at 0° through a dropping funnel. After stirring at 0° to 10° for 15 min, the mixture was heated to reflux for 1 1/2 hrs. It was then partitioned between water and benzene. The benzene layer was separated, dried and evaporated. Crystallization of the residue form methylene chloride/hexane yielded the above-named product, mp 215°-217°.

1. temperaturethe mixture was heated
2. temperatureto reflux for 1 1/2 hrs
3. customIt was then partitioned between water and benzene
4. customThe benzene layer was separated
5. customdried
6. customevaporated
7. customCrystallization of the residue form methylene chloride/hexane
8. customyielded the above-named product, mp 215°-217°