HRID47113
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
2.6 gm of a 55% suspension of sodium hydride in oil were added in portions to a mixture of 5.1 gm of 7,7-dimethyl-2-phenyl-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione hydrochloride and 50 ml of dimethyl sulfoxide. After stirring the mixture at room temperature for one hour, 4.8 gm of 3-diethylamino propyl bromide hdyrobromide were added, and the mixture was heated at 50° C. for 3 hours. The reaction mixture was admixed with water and extracted several times with chloroform. The chloroform phases were evaporated and the residue was purified on a silicagel column. The dihydrochloride was precipitated from acetone with ethereal hydrochloric acid and recrystallized from methanol/acetone.
WORKUP
后处理
- temperaturethe mixture was heated at 50° C. for 3 hours
- extractionextracted several times with chloroform
- customThe chloroform phases were evaporated
- customthe residue was purified on a silicagel column
- customThe dihydrochloride was precipitated from acetone with ethereal hydrochloric acid
- customrecrystallized from methanol/acetone