HRID2071312

反应详情

EQUATION

反应方程式

HRID 2071312 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 500 ml. electromagnetically stirred glass reactor was charged with 5.0 g (0.0167 mole) of dinitroanthraquinone (a mixture of 1,5-isomer and 1,8-isomer), 100 g (0.1 mole) of a 4% aqueous solution of sodium hydroxide and 0.25 g of 5% palladium-carbon. The inside of the reactor was purged with hydrogen, and the dinitroanthraquinone was hydrogenated at 30° C. with stirring. In 5 hours, 0.1169 mole of hydrogen was absorbed, the reaction was stopped. The reaction mixture was filtered in an atmosphere of nitrogen to separate the catalyst. Then, the filtrate was oxidized with air with stirring at 20° to 30° C. for 2 hours. The resulting crystals were filtered and dried to afford 3.9 g of diaminoanthraquinone (a mixture of 1,5-isomer and 1,8-isomer) in a yield of 97.5%.

WORKUP

后处理

  1. customThe inside of the reactor was purged with hydrogen
  2. customwas hydrogenated at 30° C.
  3. filtrationThe reaction mixture was filtered in an atmosphere of nitrogen
  4. customto separate the catalyst
  5. stirringwith stirring at 20° to 30° C. for 2 hours
  6. filtrationThe resulting crystals were filtered
  7. customdried