反应详情

A solution of 8.0 g. of [(3-dimethylcarbamoyl-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)sulfonyl]carbamic acid ethyl ester and 2.4 ml. of cyclopentylamine in 43 ml. of dioxane is heated under reflux for 1 hour and the solution subsequently evaporated in vacuo. Chromatography of the evaporation residue on 400 g. of silica gel with a mixture of 5 parts by volume of methanol and 95 parts by volume of chloroform yields the 1-cyclopentyl-3-[(3-dimethylcarbamoyl-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)sulfonyl]urea, m.p. 179°-180° C.

1. temperatureunder reflux for 1 hour
2. customthe solution subsequently evaporated in vacuo
3. additionof silica gel with a mixture of 5 parts by volume of methanol and 95 parts by volume of chloroform