HRID258059

反应详情

EQUATION

反应方程式

HRID 258059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

20 g (7.19 10-2 moles) of 4 nitro 4'bromobiphenyl, 11.6 of copper cyanide and 120 ml of DMF are placed in a 250 ml receptacle with a magnetic agitator. The mixture is refluxed for 5 h 30. It is then allowed to cool, acetone is added and the reaction medium is poured into 2 liters of water containing 2 g of ethylene diamine. A precipitate is formed. The solid is filtered out then washed in water and hexane. This raw product is redissolved in chloroform. The organic phase is dried on MgSO4, filtered and evaporated till dry. The solid obtained is recrystallized in an ethanol-chloroform mixture. This provides 13.16 g of product, yield ρ=81.7%, melting point=195° C.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 5 h 30
  2. temperatureto cool
  3. customA precipitate is formed
  4. filtrationThe solid is filtered
  5. washout then washed in water
  6. dissolutionThis raw product is redissolved in chloroform
  7. customThe organic phase is dried on MgSO4
  8. filtrationfiltered
  9. customevaporated
  10. customtill dry
  11. customThe solid obtained
  12. customis recrystallized in an ethanol-chloroform mixture