反応 #10019

反応方程式

3,4-dichlorobenzonitrile

potassium fluoride

→

3-Chloro-4-fluorobenzo-nitrile

収率 92.0%

溶媒

dimethylsulfoxide

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 6 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
   その他the 3-chloro-4-fluorobenzonitrile that precipitated
9. 9
   その他was isolated by filtration
10. 10
    洗浄washing
11. 11
    その他drying

実験手順

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.

出典