反应详情

1.5 g of 1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-hydroxy-5-methoxypyrazole was dissolved in 30 mL of N,N-dimethylformamide, 40 g of triethylamine was added, and stirring was carried out at 50° C. for 3 hours while trifluoromethyl trifluorovinyl ether was blown. To this solution, ethyl acetate was added, followed by washing with a saturated aqueous solution of citric acid, and then the organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, and the obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:4) to obtain 1.1 g of 1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-5-methoxy-3-{1,1,2-trifluoro-2-(trifluoromethoxy)ethoxy}pyrazole.

1. washby washing with a saturated aqueous solution of citric acid
2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
3. distillationthe solvent was distilled off under reduced pressure
4. customthe obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:4)