反应详情

Sodium hydride (29 mg, 60%, 0.73 mmol) was suspended in tetrahydrofuran (10 ml), and a solution of N-{3-isobutyl-4-[1-methoxy-2,2,2-trifluoro-1-(trifluoromethyl)ethyl]phenyl}-1,3,5-trimethylpyrazole-4-carboxamide (260 mg, 0.48 mmol) in tetrahydrofuran (5 ml) was added dropwise. After stirring at room temperature for 30 min, a solution of chloromethyl ethyl ether (70 mg, 0.73 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 the mixture was 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 (200 mg).

1. stirringthe mixture was stirred for one day
2. extractionthe mixture was extracted 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)