HRID258059
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture is refluxed for 5 h 30
- temperatureto cool
- customA precipitate is formed
- filtrationThe solid is filtered
- washout then washed in water
- dissolutionThis raw product is redissolved in chloroform
- customThe organic phase is dried on MgSO4
- filtrationfiltered
- customevaporated
- customtill dry
- customThe solid obtained
- customis recrystallized in an ethanol-chloroform mixture