反应详情

Sodium hydride (38 mg, 60%, 0.96 mmol) was suspended in tetrahydrofuran (10 ml), and a solution of N-{3-isobutyl-4-[2,2,2-trifluoro-1-(trifluoromethyl)ethyl]phenyl}-1,3,5-trimethylpyrazole-4-carboxamide (300 mg, 0.64 mmol) in tetrahydrofuran (5 ml) was added dropwise. After stirring at room temperature for 30 min, a solution of acetyl chloride (75 mg, 0.96 mmol) in tetrahydrofuran (2 ml) was added, and the mixture was stirred for one day. The reaction mixture was poured into diluted hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with water, dried over magnesium sulfate and concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:3) to give the desired compound (90 mg).

1. stirringthe mixture was stirred for one day
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:3)