HRID47112

反应详情

EQUATION

反应方程式

HRID 47112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.2 gm of 2,7,7-trimethyl-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione were dissolved in 100 ml of dimethylformamide, and the solution was admixed with 3.4 gm of diethylamino ethyl chloride hydrochloride and 4.1 gm of potassium carbonate. The mixture was refluxed for 8 hours, the solvent was distilled off in vacuo, the residue was admixed with water and extracted with chloroform. The chloroform phase was evaporated and the residue was purified on a silicagel column (eluant: chloroform/acetone 19:1). The dihydrochloride was precipitated from acetone/methanol with ethereal hydrochloric acid and recrystallized from acetone/methanol.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 8 hours
  2. distillationthe solvent was distilled off in vacuo
  3. extractionextracted with chloroform
  4. customThe chloroform phase was evaporated
  5. customthe residue was purified on a silicagel column (eluant: chloroform/acetone 19:1)
  6. customThe dihydrochloride was precipitated from acetone/methanol with ethereal hydrochloric acid
  7. customrecrystallized from acetone/methanol