反应详情

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
4. waitAfter standing overnight
5. temperaturethe reaction was heated to 110 C
6. waitfor an additional four hours
7. temperatureto cool to 50 C
8. waitThen 19.0 g of thionyl chloride was dropwise over fifteen minutes
9. temperatureThe reaction was then heated to 80 C
10. waitfor twenty minutes
11. waitfor one hour
12. temperatureAfter cooling
13. additionthe reaction was cautiously added to 600 g of ice
14. extractionThe aqueous phase was extracted with two 250 ml portions of ether
15. dry with materialThe combined organic extracts were dried with MgSO4
16. concentrationconcentrated under reduced pressure