反应详情

Acetic acid (5 mL) was added to a solution of 4-mesityl-3-methyl-1H-5-pyrazoleamine (5 g, 23.22 mmol) and diethyl 2-acetylmalonate (4.7 g, 23.22 mmol) in xylene (40 mL), followed by heating under reflux for seven hours. The reaction mixture was evaporated as it was, and water was added thereto. After extracting with ethyl acetate, the organic layer was washed with an aqueous saturated sodium bicarbonate and brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (20% ethyl acetate/hexane), to give the title compound (3 g).

1. temperatureby heating
2. temperatureunder reflux for seven hours
3. customThe reaction mixture was evaporated as it
4. additionwater was added
5. extractionAfter extracting with ethyl acetate
6. washthe organic layer was washed with an aqueous saturated sodium bicarbonate and brine
7. dry with materialdried over anhydrous magnesium sulfate
8. customevaporated
9. customThe residue was purified by silica gel column chromatography (20% ethyl acetate/hexane)