反应详情

A suspension of 1.20 g (3.14 mmol) of 7-chloro-3-(5-chloromethyl-1,2,4-oxadiazol-3-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one in 20 ml of N,N-dimethylformamide was treated with 1.59 g (0.0166 mol) of diisopropylamine. After stirring at 80° for 20 hrs. the solution obtained was completely freed from the solvents. The residue was chromatographed over silica gel with methylene chloride/methanol 39:1 as the eluent. The product was recrystallized from ether/n-hexane. There was obtained 0.84 g (60%) of 7-chloro-3-(5-diisopropylaminomethyl-1,2,4-oxadiazol-3-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one as whitish crystals; m.p. 153°-156°.

1. customthe solution obtained
2. customThe residue was chromatographed over silica gel with methylene chloride/methanol 39:1 as the eluent
3. customThe product was recrystallized from ether/n-hexane