HRID47107

反应详情

EQUATION

反应方程式

HRID 47107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

5.1 gm of 7,7-dimethyl-2-(2-methoxy-4-methylmercapto-phenyl)-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione were reacted in 100 ml of 70% acetic acid with 1.7 gm of 30% hydrogen peroxide, and the mixture was allowed to stand for 50 hours at room temperature (the first 3 hours while stirring). After 18 and again after 26 hours 1.3 gm of 30% hydrogen peroxide were added. The reaction mixture was then diluted with water, and ammonia was added until alkaline reaction. The precipitate was suction-filtered off and the filtrate was extracted twice with chloroform. The combined chloroform phases were evaporated, and the evaporation residue was combined with the precipitate. The thus obtained product was purified on a silicagel column (eluant: chloroform/acetone 19:1).

WORKUP

后处理

  1. additionwas added until alkaline reaction
  2. filtrationThe precipitate was suction-filtered off
  3. extractionthe filtrate was extracted twice with chloroform
  4. customThe combined chloroform phases were evaporated
  5. customThe thus obtained product was purified on a silicagel column (eluant: chloroform/acetone 19:1)