反应详情

温度

122.5 °C

4-Iodo-3-pentafluoroethyl-1H-pyrazole (12.48 g), copper powder (7.63 g), iodopentafluoroethane (29.50 g) and DMF (60 ml) were set in an autoclave and heated and stirred for 8 hours, maintaining the inside temperature of 120-125° C. After cooling to room temperature, the insoluble material was filtered off through Celite and washed with diethyl ether. The filtrate was diluted with water and extracted with diethyl ether. The organic phase was washed with water and dried over sodium sulfate, and concentrated under the reduced pressure. The crude product was distilled under reduced pressure to obtain 3,4-bis-pentafluoroethyl-1H-pyrazole (1.20 g), bp. 110-115° C./20 mbar.

1. temperatureheated
2. temperatureAfter cooling to room temperature
3. filtrationthe insoluble material was filtered off through Celite
4. washwashed with diethyl ether
5. additionThe filtrate was diluted with water
6. extractionextracted with diethyl ether
7. washThe organic phase was washed with water
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated under the reduced pressure
10. distillationThe crude product was distilled under reduced pressure