HRID47113

反应详情

EQUATION

反应方程式

HRID 47113 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe mixture was heated at 50° C. for 3 hours
  2. extractionextracted several times with chloroform
  3. customThe chloroform phases were evaporated
  4. customthe residue was purified on a silicagel column
  5. customThe dihydrochloride was precipitated from acetone with ethereal hydrochloric acid
  6. customrecrystallized from methanol/acetone