反应详情

To a stirred solution of 915 mg (3.0 mmoles) of 7-chloro-5-(2-chlorophenyl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one in 10 ml of dry tetrahydrofuran was added 173 mg of a 50% dispersion as sodium hydride in oil (3.6 mmoles of hydride). The mixture was stirred at room temperature approximately 1 hr until hydrogen evolution stopped. Dimorpholinophosphinic chloride (1.5 g; 6.0 mmoles) was added and the resulting mixture was stirred at room temperature for 2 hrs. Insoluble salts were removed by filtration. Tetrahydrofuran was evaporated. The residue was crystallized from ethyl acetate to give colorless needles, mp 185°-187°.

1. customInsoluble salts were removed by filtration
2. customTetrahydrofuran was evaporated
3. customThe residue was crystallized from ethyl acetate
4. customto give colorless needles, mp 185°-187°