反応 #10018

反応方程式

4-nitrochlorobenzene

potassium fluoride

→

4-nitrofluorobenzene

収率 96.0%

溶媒

dimethylsulfoxide

反応条件

後処理

1. 1
   その他equipped with thermometer, anchor stirrer
2. 2
   温度reflux condenser
3. 3
   その他with bubble counter
4. 4
   温度The mixture was heated
5. 5
   温度The reaction mixture was then cooled to room temperature
6. 6
   workup.ADDITIONwater was added at a volumetric ratio of 1:1
7. 7
   その他the phases that formed
8. 8
   その他were separated
9. 9
   workup.DISTILLATIONfrom the organic phase, by fractional distillation at reduced pressure

実験手順

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.

出典