HRID47120

反应详情

EQUATION

反应方程式

HRID 47120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture consisting of 1.5 gm of 7,7-dimethyl-2-(4-chlorophenyl)-5-(2-chloro-ethyl)-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione and 1.7 gm of N-methyl-N-(2-(3,4-dimethoxy-phenyl)-ethyl)-amine was heated at 150° C. for 3 hours. After cooling the reaction mixture was dissolved in chloroform, and the solution was washed with water. The chloroform phase was evaporated, and the residue was chromatographed on a silicagel column (eluant: chloroform/acetone 19:1). The dihydrochloride was precipitated from acetone by addition of ethereal hydrochloric acid and recrystallized from methylene chloride/acetone.

WORKUP

后处理

  1. temperatureAfter cooling the reaction mixture
  2. washthe solution was washed with water
  3. customThe chloroform phase was evaporated
  4. customthe residue was chromatographed on a silicagel column (eluant: chloroform/acetone 19:1)
  5. customThe dihydrochloride was precipitated from acetone by addition of ethereal hydrochloric acid
  6. customrecrystallized from methylene chloride/acetone