HRID47120
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling the reaction mixture
- washthe solution was washed with water
- customThe chloroform phase was evaporated
- customthe residue was chromatographed on a silicagel column (eluant: chloroform/acetone 19:1)
- customThe dihydrochloride was precipitated from acetone by addition of ethereal hydrochloric acid
- customrecrystallized from methylene chloride/acetone