反应详情

A solution of 1.75 g of 4-chloroacetyl-1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one and 1.15 g of N-methylpiperazine in 50 ml of dry dioxane is warmed at 50° C. for 5 hours with stirring. After the mixture has cooled, the precipitate formed is filtered off. The filtrate is concentrated, 50 ml of saturated sodium bicarbonate solution are added, and the thus-prepared mixture is extracted several times with ethyl acetate. The combined extracts are dried over sodium sulfate and concentrated. 1.5 g of the title compound of m.p. 205° to 207° C. (from ethyl acetate) are obtained. M.p. of the dihydrochloride: 212° C. (D., from water). M.p. of the hemifumarate: 173° C. (from ethanol).

1. temperatureAfter the mixture has cooled
2. customthe precipitate formed
3. filtrationis filtered off
4. concentrationThe filtrate is concentrated
5. addition50 ml of saturated sodium bicarbonate solution are added
6. extractionthe thus-prepared mixture is extracted several times with ethyl acetate
7. dry with materialThe combined extracts are dried over sodium sulfate
8. concentrationconcentrated