HRID1587257

反应详情

EQUATION

反应方程式

HRID 1587257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 5 liter-reaction vessel, 100 g (5.32×10-1M) of 2,5-dicyano-1,4-dimethoxybenzene, 312.5 g (1.17 M) of anhydrous aluminum tribromide and 2.5 liters of dry benzene were placed, followed by heat-refluxing for 7 hours. After the reaction, the reaction mixture as cooled and poured into a mixture of 3 kg of crushed ice and 500 ml of concentrated hydrochloric acid to precipitate a crystal. The crystal was recovered by filtration and dissolved in 2N-sodium hydroxide aqueous solution. The resultant insoluble residue was filtered off and the filtrate was acidified with 2N-hydrochloric acid to precipitate a crystal. The crystal was recovered by filtration and washed with water, followed by drying to obtain 35.5 g of 2,5-dicyanohydroquinone (Yield: 41.7%).

WORKUP

后处理

  1. temperatureby heat-refluxing for 7 hours
  2. customAfter the reaction
  3. temperaturethe reaction mixture as cooled
  4. customto precipitate a crystal
  5. filtrationThe crystal was recovered by filtration
  6. dissolutiondissolved in 2N-sodium hydroxide aqueous solution
  7. filtrationThe resultant insoluble residue was filtered off
  8. customto precipitate a crystal
  9. filtrationThe crystal was recovered by filtration
  10. washwashed with water
  11. customby drying