HRID499218

反应详情

EQUATION

反应方程式

HRID 499218 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, under an inert atmosphere, into a 500 ml three-necked flask equipped with a Dean-Starck apparatus and a condenser. 90 ml of DMF and 110 ml of toluene are added. The medium is heated to 140° C. under nitrogen; 80 ml of toluene are distilled. The medium is then cooled to AT and then deoxygenated with nitrogen bubbling. 6 g of iodoanisole are then added and the medium is heated at 155° C. for 20 h. After a return to AT, the medium is diluted in 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 a Dean-Starck apparatus and a condenser
  2. distillation80 ml of toluene are distilled
  3. temperatureThe medium is then cooled to AT
  4. customdeoxygenated with nitrogen bubbling
  5. addition6 g of iodoanisole are then added
  6. temperaturethe medium is heated at 155° C. for 20 h
  7. additionAfter a return to AT, the medium is diluted in 200 ml of a water/ethyl ether mixture
  8. filtrationThe medium is then filtered through Celite®
  9. washThe organic phase is washed 3 times with water
  10. dry with materialdried over MgSO4
  11. customevaporated