反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customequipped with Dean-Stark apparatus and a condenser, under an inert atmosphere
- distillation80 ml of toluene are distilled off
- temperatureThe medium is then cooled to RT
- customdeoxygenated
- customby sparging with nitrogen
- addition6 g of iodoanisole are then added
- temperatureby heating at 155° C. for 20 hours
- temperatureAfter cooling to RT
- additionthe medium is diluted with 200 ml of a water/ethyl ether mixture
- filtrationThe medium is then filtered through Celite®
- washThe organic phase is washed 3 times with water
- dry with materialdried over MgSO4
- customevaporated