反应详情

9.8 g (32.1 mmol) of 7-chloro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]-benzodiazepine-3-carboxamidoxime were stirred with 7 g (41 mmol) of chloroacetic anhydride in 60 ml of N,N-dimethylformamide at room temperature for 1 hour and at 105° for 4 hours. After evaporating the reaction mixture the residue was dissolved in methylene chloride and the solution was washed with saturated sodium bicarbonate solution. The organic phase was dried over magnesium sulfate and concentrated, and the residue was chromatographed on silica gel while eluting with ethyl acetate. There were obtained 6.63 g (57%) of 7-chloro-3-(5-chloromethyl-1,2,4-oxadiazol-3-yl)-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one of m.p. 208°-210°.

1. customAfter evaporating the reaction mixture the residue
2. dissolutionwas dissolved in methylene chloride
3. washthe solution was washed with saturated sodium bicarbonate solution
4. dry with materialThe organic phase was dried over magnesium sulfate
5. concentrationconcentrated
6. customthe residue was chromatographed on silica gel
7. washwhile eluting with ethyl acetate