反应详情

7.5 g of 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepine-2-thione are suspended in 125 ml of dioxane and 50 ml of dimethylformamide and 2.2 g of sodium bicarbonate and 1.8 g of hydroxylammonium chloride are added to the suspension. After stirring for 8 hours at room temperature (monitoring by thin layer chromatography), the mixture is filtered off under suction and 2.8 ml of phenylisocyanate are added to the filtrate. After stirring for 30 minutes, the reaction mixture is added dropwise into 200 ml of water and the mixture is filtered off under suction. Recrystallization from ethanol/dimethylformamide yields colorless crystals of melting point 215°-217° C. Yield 4.6 g.

1. filtrationthe mixture is filtered off under suction and 2.8 ml of phenylisocyanate
2. additionare added to the filtrate
3. stirringAfter stirring for 30 minutes
4. additionthe reaction mixture is added dropwise into 200 ml of water
5. filtrationthe mixture is filtered off under suction
6. customRecrystallization from ethanol/dimethylformamide
7. customyields colorless crystals of melting point 215°-217° C