反应详情

A suspension of 1.30 g (0.0037 mol) of 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 15 ml of dimethylformamide was treated with 2.4 g (0.01 9 moll of dibutylamine. After stirring at room temperature for 65 hrs. the orange solution obtained was freed completely from solvent. The residue was chromatographed over silica gel with dichloromethane/methanol 19:1 as the eluent. The product was recrystallized from methanol/ether and there were obtained 1.27 g (77%) of 3-(5-dibutylaminomethyl-1,2,4-oxadiazol-3-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one as white crystals; m.p. 137°-140°.

1. customthe orange solution obtained
2. customThe residue was chromatographed over silica gel with dichloromethane/methanol 19:1 as the eluent
3. customThe product was recrystallized from methanol/ether