反应详情

A solution of ethyl 1-butyl-5-methyl-1H-pyrazole-3-carboxylate (18.1 g, 86.1 mmol) in methanol (25 mL) was treated with ammonium hydroxide (25 mL) according to a modification of the method described in Part D of Examples 1-4. At the end of the reaction, the methanol was removed under reduced pressure, and the remaining solution was cooled in a refrigerator. A precipitate formed, was isolated by filtration, and was washed with water. The solid (9 g) was recrystallized from hexane (300 mL) and ethyl acetate (30 mL), isolated by filtration, washed with hexane, and air-dried to provide 6.95 g of 1-butyl-5-methyl-1H-pyrazole-3-carboxamide as colorless plates, mp 113.5-114.5° C.

1. customAt the end of the reaction
2. customthe methanol was removed under reduced pressure
3. temperaturethe remaining solution was cooled in a refrigerator
4. customA precipitate formed
5. customwas isolated by filtration
6. washwas washed with water
7. customThe solid (9 g) was recrystallized from hexane (300 mL) and ethyl acetate (30 mL)
8. customisolated by filtration
9. washwashed with hexane
10. customair-dried