반응 #10019

반응 방정식

3,4-dichlorobenzonitrile

potassium fluoride

→

3-Chloro-4-fluorobenzo-nitrile

수율 92.0%

용매

dimethylsulfoxide

반응 조건

후처리

1. 1
   기타equipped with anchor stirrer
2. 2
   온도thermometer, and reflux condenser
3. 3
   기타with bubble counter
4. 4
   온도The mixture was then heated
5. 5
   온도this temperature was maintained for 6 hours
6. 6
   온도The 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
   기타the 3-chloro-4-fluorobenzonitrile that precipitated
9. 9
   기타was isolated by filtration
10. 10
    세척washing
11. 11
    기타drying

실험 절차

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.

출처