HRID2071316

反应详情

EQUATION

反应方程式

HRID 2071316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2.5 g (0.01 mole) of 2-nitroanthraquinone (purity above 99%) containing about 10% of particles having a particle diameter of more than 100 microns was placed in a 200 ml. electromagnetically stirred autoclave together with 25 g of small glass balls each with a diameter of 1 mm, 75 g of water and 0.025 g of 5% palladium-carbon. The inside of the autoclave was purged with hydrogen, and then, the 2-nitroanthraquinone was hydrogenated with stirring at a temperature of 100° C. and a pressure of 2 to 6 Kg/cm2.G. The reaction proceeded smoothly, and stopped in 4 hours with the absorption of a theoretical amount of hydrogen. The reaction mixture was filtered, and the 22 g of conc. sulfuric acid was added to the filtrate mass to dissolve the reaction product. Then, the catalyst and the small glass balls were separated by filtration. The filtrate was diluted with water. The precipitated crystals were collected by filtration to afford 2.2 g of 2-aminoanthraquinone. The purity of the product was 99%, and its yield was almost quantitative.

WORKUP

后处理

  1. customThe inside of the autoclave was purged with hydrogen
  2. customstopped in 4 hours with the absorption of a theoretical amount of hydrogen
  3. filtrationThe reaction mixture was filtered
  4. additionthe 22 g of conc. sulfuric acid was added to the filtrate mass
  5. dissolutionto dissolve the reaction product
  6. customThen, the catalyst and the small glass balls were separated by filtration
  7. additionThe filtrate was diluted with water
  8. filtrationThe precipitated crystals were collected by filtration