HRID850902

反应详情

EQUATION

反应方程式

HRID 850902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

250 ml of quinoline, 100 g of 1-aminoanthraquinone and 25 g of CaO are warmed to 200° to 210° C. in a 1 l sulphonation beaker with an anchor stirrer and shortpath distillation bridge. 120 g of 1-nitroanthraquinone are added in portions in the course of 2 hours, and the mixture is then stirred for another 5 hours at 200° to 210° C. The mixture is allowed to cool to 120° C., and is diluted slowly and under reflux with 500 ml of ethanol. The mixture is then filtered off under suction, and the residue is washed with ethanol and dried. The dry caked filter residue is heated under reflux in 1 l of water with 100 g of ammonium chloride, and is acidified slowly through the reflux condenser with concentrated hydrochloric acid. After filtering off the mixture under suction, washing the residue until the runnings are neutral, and drying, 190.4 g of 80.4% strength 1,1'-dianthraquinonylamine are obtained.

WORKUP

后处理

  1. additionis diluted slowly
  2. filtrationThe mixture is then filtered off under suction
  3. washthe residue is washed with ethanol
  4. customdried
  5. temperatureThe dry caked filter residue is heated
  6. temperatureunder reflux in 1 l of water with 100 g of ammonium chloride
  7. filtrationAfter filtering off the mixture under suction
  8. washwashing the residue until the runnings
  9. customdrying