HRID745307

反应详情

EQUATION

反应方程式

HRID 745307 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 9,10-dimethoxy-2-chloro-6,7-dihydro-4H-pyrimido(6,1-a)isoquinolin-4-one (3.0 g) and tert.-butylamine (10.0 ml) in chloroform (75 ml) is heated under reflux for 16 hours. The solvent is evaporated under reduced pressure and the residue triturated with a dilute solution of sodium hydroxide to give a white precipitate. The precipitate is filtered, dried and converted into its hydrochloride by treating it in solution in ethanol with hydrochloric acid. The hydrochloride is crystallized from ethanol-ether mixture, yield 3.0 g, m.p. 265°-270° C.

WORKUP

后处理

  1. temperatureunder reflux for 16 hours
  2. customThe solvent is evaporated under reduced pressure
  3. customthe residue triturated with a dilute solution of sodium hydroxide
  4. customto give a white precipitate
  5. filtrationThe precipitate is filtered
  6. customdried
  7. additionby treating it in solution in ethanol with hydrochloric acid
  8. customThe hydrochloride is crystallized from ethanol-ether mixture, yield 3.0 g, m.p. 265°-270° C.