HRID2216778

反应详情

EQUATION

反应方程式

HRID 2216778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of the methyl 3-chloro-5-fluorobenzoate, zinc cyanide (8.46 g, 72.3 mmol) zinc (dust, 235 mg, 3.6 mmol), [1,1′bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with dichloromethane (1:1) (1.5 g, 1.8 mmol) in N,N-dimethylformamide (70 ml) was heated at reflux for 1 hour. The reaction was cooled to ambient temperature and diluted with ethyl acetate. The organic solution was extracted with water and brine and concentrated in vacuo, to afford crude methyl 3-chloro-5-cyanobenzoate.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 1 hour
  3. extractionThe organic solution was extracted with water and brine
  4. concentrationconcentrated in vacuo