HRID226251

反应详情

EQUATION

反应方程式

HRID 226251 的结构方程式

PROCEDURE

实验过程

To crude 1,5-diamino-4,8-dihydroxyanthraquinone (11 g, 0.041 mol) was added NaOH (2.5 M, 200 mL) and the suspension was refluxed gently for 3 hours before it was allowed to cool down to room temperature. Sodium hydrogen sulphite (31.74 g, 0.182 mol) was added portionwise and the reaction mixture was refluxed again for 3 hours. It was cooled down to room temperature and was acidified with concentrated hydrochloric acid until pH 3. The precipitate was isolated by filtration and washed successively with cold water and then hot water. After lyophilisation overnight, the title compound was afforded as a crude brown solid (8 g, 73%). FAB MS, m/z(M+H)+ 251.

WORKUP

后处理

  1. temperaturethe suspension was refluxed gently for 3 hours before it
  2. temperaturethe reaction mixture was refluxed again for 3 hours
  3. temperatureIt was cooled down to room temperature
  4. customThe precipitate was isolated by filtration
  5. washwashed successively with cold water