HRID47112
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
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
- temperatureThe mixture was refluxed for 8 hours
- distillationthe solvent was distilled off in vacuo
- extractionextracted with chloroform
- customThe chloroform phase was evaporated
- customthe residue was purified on a silicagel column (eluant: chloroform/acetone 19:1)
- customThe dihydrochloride was precipitated from acetone/methanol with ethereal hydrochloric acid
- customrecrystallized from acetone/methanol