反应详情

A solution of 9,10-dimethoxy-6,7-dihydro-2-chloro-4H-pyrimido(6,1-a)isoquinolin-4-one (2.5 g), sec-butylamine (10 ml) and dimethylformamide (2 ml) is heated under reflux for 5 hours. The solvent and excess amine are distilled under reduced pressure. The residue is treated with water. A white solid precipitates and is collected by filtration. The precipitate is crystallized from methylene chloride-ether mixture, yield 2.10 g. The crystals are dissolved in dichloromethane and treated with a solution of etheral hydrochloric acid. The hydrochloride is crystallized from ethanol-ether mixture, m.p. 218°-225° C.

1. temperatureunder reflux for 5 hours
2. distillationThe solvent and excess amine are distilled under reduced pressure
3. additionThe residue is treated with water
4. customA white solid precipitates
5. filtrationis collected by filtration
6. customThe precipitate is crystallized from methylene chloride-ether mixture, yield 2.10 g
7. dissolutionThe crystals are dissolved in dichloromethane
8. additiontreated with a solution of etheral hydrochloric acid
9. customThe hydrochloride is crystallized from ethanol-ether mixture, m.p. 218°-225° C.