反応 #10020

反応方程式

4-chlorobenzonitrile

potassium fluoride

→

4-fluorobenzo-nitrile

収率 75.0%

溶媒

dimethyl sulfoxide

反応条件

後処理

1. 1
   その他equipped with anchor stirrer
2. 2
   温度thermometer, and reflux condenser
3. 3
   その他with bubble counter
4. 4
   温度The mixture was then heated
5. 5
   温度this temperature was maintained for 16 hours
6. 6
   温度The mixture was then cooled to room temperature
7. 7
   workup.ADDITIONwater was added to the reaction mixture in a volumetric ratio of 1:1
8. 8
   抽出the mixture was extracted with diethyl ether
9. 9
   洗浄After washing
10. 10
    濃縮concentration
11. 11
    その他drying the separated organic phase

実験手順

200 g of 4-chlorobenzonitrile, 101.4 g of potassium fluoride, 25 g of dimethyl sulfoxide, and 5.60 g of (N,N-dimethylimidazolidino)tetramethyl-guanidinium chloride were placed in a 1 liter 4-neck flask equipped with anchor stirrer, thermometer, and reflux condenser with bubble counter. The mixture was then heated with stirring to 180° C. and this temperature was maintained for 16 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 mixture was extracted with diethyl ether. After washing, concentration, and drying the separated organic phase, 4-fluorobenzo-nitrile was isolated in a yield of 75%.

出典