反应详情

温度

110 °C

To 53 mls of chlorosulfonic acid at 10° C. was added dropwise over fifteen minutes 1,5-dimethyl-3-(trifluoromethyl)pyrazole (24.0 grams). No significant exotherm resulted and after 15 minutes the cooling bath was removed and the reaction was heated to 110° C. for three hours. After standing overnight, the reaction was heated to 110° C. for an additional four hours and allowed to cool to 50° C. Then 19.0 g of thionyl chloride was dropwise over fifteen minutes. The reaction was then heated to 80° C. for twenty minutes and 110° C. for one hour. After cooling, the reaction was cautiously added to 600 g of ice. The aqueous phase was extracted with two 250 ml portions of ether. The combined organic extracts were dried with MgSO4 and concentrated under reduced pressure to yield 7.8 g of the desired product as a tan oil.

1. customNo significant exotherm resulted and after 15 minutes the cooling bath
2. customwas removed
3. temperaturethe reaction was heated to 110° C. for an additional four hours
4. temperatureto cool to 50° C
5. waitThen 19.0 g of thionyl chloride was dropwise over fifteen minutes
6. temperatureThe reaction was then heated to 80° C. for twenty minutes and 110° C. for one hour
7. temperatureAfter cooling
8. additionthe reaction was cautiously added to 600 g of ice
9. extractionThe aqueous phase was extracted with two 250 ml portions of ether
10. dry with materialThe combined organic extracts were dried with MgSO4
11. concentrationconcentrated under reduced pressure