反应详情

1.65 g (5 mmol) of 3-(5-chloromethyl-1,2,4-oxadiazol-3-yl)-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one were stirred at 75° for 24 hours in 3 ml (17.5 mmol) of di-sec.-butylamine and 25 ml of N,N-dimethylformamide. By evaporation of the reaction mixture and chromatography of the residue on silica gel while eluting with methylene chloride/methanol 19/1 and crystallization from ethyl acetate there were obtained 1.23 g (58%) of 3-(5-di-sec.-butylaminomethyl-1,2,4-oxadiazol-3-yl)-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]-benzodiazepin-6-one of m.p. 155°-157°, which was converted into the hydrochloride of m.p. 133°-140°.

1. customBy evaporation of the reaction mixture and chromatography of the residue on silica gel
2. washwhile eluting with methylene chloride/methanol 19/1 and crystallization from ethyl acetate