反应详情

7.47 g (20 mmol) of 7-chloro-4,5-dihydro-3-iodo-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepine-6-one were heated to boiling under reflux for 4 hours with 1.75 g (25 mmol) of 3-butyn-2-ol, 70 mg of bis-(triphenyl -phosphine)-palladium(II) dichloride and 10 mg of copper(I) iodide in 50 ml of diethylamine and 20 ml of ethylene chloride. After evaporation of the solvent the residue was taken up in methylene chloride and the resulting suspension was suction filtered. The material obtained was washed with methylene chloride and, after recrystallization from ethyl acetate, there was obtained 7-chloro -4,5-dihydro-3-(3-hydroxy-1-butynyl)-5-methyl-6H-imidazo -[1,5-a][1,4]benzodiazepin-6-one of melting point 251-252° C.

1. customAfter evaporation of the solvent the residue
2. filtrationsuction filtered
3. customThe material obtained
4. washwas washed with methylene chloride
5. customafter recrystallization from ethyl acetate