反应详情

To a solution of 610 mg. (2 mmoles) of 7-chloro-5-(2-chlorophenyl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one in 10 ml. of dry tetrahydrofuran at room temperature was added 115 mg. of a 50% dispersion of sodium hydride in oil (2.4 mmoles of hydride). The mixture was warmed gently on the steam bath for approximately 1 hour until hydrogen evolution stopped. Dimorpholinophosphinic chloride (764 mg., 3.0 mmoles) was added and the resulting mixture was stirred at room temperature for 2 hours. To this mixture was then added a solution of 296 mg. (4 mmoles) of acethydrazide in 5 ml. of dry tetrahydrofuran and stirring was continued for 15 minutes at room temperature. Solvents were evaporated and the residue was dissolved in 20 ml. of butanol and heated to reflux for 2 hours. Butanol was evaporated. The residue was partitioned between methylene chloride and water. The methylene chloride layer was dried and evaporated. Crystallization of the residue from isopropanol-ether-petroleum ether yielded, in two crops, final product having a m.p. of 225°-227°.

1. additionTo this mixture was then added a solution of 296 mg
2. waitwas continued for 15 minutes at room temperature
3. customSolvents were evaporated
4. dissolutionthe residue was dissolved in 20 ml
5. temperatureof butanol and heated
6. temperatureto reflux for 2 hours
7. customButanol was evaporated
8. customThe residue was partitioned between methylene chloride and water
9. dry with materialThe methylene chloride layer was dried
10. customevaporated
11. customCrystallization of the residue from isopropanol-ether-petroleum ether