HRID1685400

反应详情

EQUATION

反应方程式

HRID 1685400 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

10 g (35.96 mM) of (4-bromophenyl)(3-hydroxy-2-pyridinyl)methanone are mixed with 6.44 g (71.92 mM) of cuprous cyanide in 90 ml of dimethylformamide. The mixture is refluxed for 21 h. A solution of 19.25 g of ferric chloride in 42.5 ml of water and 6.7 ml of concentrated hydrochloric acid is prepared and added to the cooled reaction medium and the resulting mixture is then heated at 90° C. for 30 minutes. After cooling, ethyl acetate and water are added and the mixture is filtered on Celite. The product is then extracted with ethyl acetate and the organic phase is washed with saturated sodium chloride solution. The solvent is evaporated off under reduced pressure to give the desired product in the form of a yellow solid with a yield of 45%.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 21 h
  2. additionadded to the cooled reaction medium
  3. temperatureAfter cooling
  4. filtrationthe mixture is filtered on Celite
  5. extractionThe product is then extracted with ethyl acetate
  6. washthe organic phase is washed with saturated sodium chloride solution
  7. customThe solvent is evaporated off under reduced pressure