HRID1461092
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
8.13 g of CuCN are added to a solution of 5.1 g of 4,4'-dibromobenzophenone in 90 ml of DMF and the mixture is stirred under reflux for 13 hours. After cooling, the reaction mixture is diluted with ethyl acetate, washed twice with 50% aqueous ethylenediamine solution, twice with water and then three times with brine, dried and concentrated. Column chromatography (SiO2, toluene to toluene/ethyl acetate 95:5) yields the crystalline title compound; TLC (toluene/ethyl acetate 9:1): Rf =0.34; IR (CH2Cl2): 2220, 1670, 1605, 1405 cm-1.
WORKUP
后处理
- temperatureunder reflux for 13 hours
- temperatureAfter cooling
- washwashed twice with 50% aqueous ethylenediamine solution, twice with water
- dry with materialthree times with brine, dried
- concentrationconcentrated