HRID504058

反应详情

EQUATION

反应方程式

HRID 504058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

8.3 g of potassium pentafluoropropionate and 9.8 g of CuI are introduced into a 500 ml three-necked flask equipped with Dean-Stark apparatus and a condenser, under an inert atmosphere. 90 ml of DMF and 110 ml of toluene are added. The medium is heated to 140° C. under nitrogen and 80 ml of toluene are distilled off. The medium is then cooled to RT and then deoxygenated by sparging with nitrogen. 6 g of iodoanisole are then added, followed by heating at 155° C. for 20 hours. After cooling to RT, the medium is diluted with 200 ml of a water/ethyl ether mixture. The medium is then filtered through Celite®. The organic phase is washed 3 times with water, dried over MgSO4 and then evaporated to give 4.3 g of a brown oil.

WORKUP

后处理

  1. customequipped with Dean-Stark apparatus and a condenser, under an inert atmosphere
  2. distillation80 ml of toluene are distilled off
  3. temperatureThe medium is then cooled to RT
  4. customdeoxygenated
  5. customby sparging with nitrogen
  6. addition6 g of iodoanisole are then added
  7. temperatureby heating at 155° C. for 20 hours
  8. temperatureAfter cooling to RT
  9. additionthe medium is diluted with 200 ml of a water/ethyl ether mixture
  10. filtrationThe medium is then filtered through Celite®
  11. washThe organic phase is washed 3 times with water
  12. dry with materialdried over MgSO4
  13. customevaporated