HRID9923

反应详情

EQUATION

反应方程式

HRID 9923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

172 g of 3,4-dichlorobenzonitrile, 200 g of dimethylsulfoxide, 69.6 g of potassium fluoride, and 3.95 g of (N,N-dimethylimidazolidino)tris-(diethylamino)phosphazenium chloride were placed in a 1 liter four-neck flask equipped with anchor stirrer, thermometer, and reflux condenser with bubble counter. The mixture was then heated with stirring to 170° C. and this temperature was maintained for 6 hours. The mixture was then cooled to room temperature, water was added to the reaction mixture in a volumetric ratio of 1:1, and the 3-chloro-4-fluorobenzonitrile that precipitated was isolated by filtration, washing, and drying. 3-Chloro-4-fluorobenzo-nitrile was obtained in a yield of 92% of theory.

WORKUP

后处理

  1. customequipped with anchor stirrer
  2. temperaturethermometer, and reflux condenser
  3. customwith bubble counter
  4. temperatureThe mixture was then heated
  5. temperaturethis temperature was maintained for 6 hours
  6. temperatureThe mixture was then cooled to room temperature
  7. additionwater was added to the reaction mixture in a volumetric ratio of 1:1
  8. customthe 3-chloro-4-fluorobenzonitrile that precipitated
  9. customwas isolated by filtration
  10. washwashing
  11. customdrying