반응 #10018

반응 방정식

4-nitrochlorobenzene

potassium fluoride

→

4-nitrofluorobenzene

수율 96.0%

용매

dimethylsulfoxide

반응 조건

후처리

1. 1
   기타equipped with thermometer, anchor stirrer
2. 2
   온도reflux condenser
3. 3
   기타with bubble counter
4. 4
   온도The mixture was heated
5. 5
   온도The reaction mixture was then cooled to room temperature
6. 6
   workup.ADDITIONwater was added at a volumetric ratio of 1:1
7. 7
   기타the phases that formed
8. 8
   기타were separated
9. 9
   workup.DISTILLATIONfrom the organic phase, by fractional distillation at reduced pressure

실험 절차

157 g of 4-nitrochlorobenzene, 200 g of dimethylsulfoxide, 62.7 g of potassium fluoride, and 2.49 g of (N,N-dimethylimidazolidino)tetramethyl-guanidinium chloride were placed in a 1 liter four-neck flask equipped with thermometer, anchor stirrer, and reflux condenser with bubble counter. The mixture was heated with stirring to 170° C. and kept at this temperature for 5 hours. The reaction mixture was then cooled to room temperature, water was added at a volumetric ratio of 1:1, the phases that formed were separated, and, from the organic phase, by fractional distillation at reduced pressure, 4-nitrofluorobenzene was obtained in a yield of 96% of theory.

출처