HRID1461092

反应详情

EQUATION

反应方程式

HRID 1461092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureunder reflux for 13 hours
  2. temperatureAfter cooling
  3. washwashed twice with 50% aqueous ethylenediamine solution, twice with water
  4. dry with materialthree times with brine, dried
  5. concentrationconcentrated