反应详情

To a suspension of 0.13 g of 60% oily sodium hydride in 10 ml of anhydrous tetrahydrofuran was added dropwise 0.7 g of 3-(2,6-dichloro-4-trifluoromethylphenyl)-1-methyl-5-mercaptopyrazole (2) in 2.0 ml of anhydrous tetrahydrofuran at 0° C., and the mixture was stirred at room temperature for 1 hour. Subsequently, with addition of an excess of trifluoromethyl iodide, the mixture was stirred for 4 hours as contained in a sealed container. Ice water was added to the reaction mixture, the mixture was thereafter extracted with ethyl acetate, and the extracts were combined together, washed with brine and dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain a residue, which was then purified by column chromatography on silica gel (eluent: ethyl acetate/hexane=1/5), giving 0.6 g of the desired compound in the form of a colorless oil (yield 48.6%).

1. stirringthe mixture was stirred for 4 hours
2. extractionthe mixture was thereafter extracted with ethyl acetate
3. washwashed with brine
4. dry with materialdried over magnesium sulfate
5. distillationThe solvent was distilled off under reduced pressure
6. customto obtain a residue, which
7. customwas then purified by column chromatography on silica gel (eluent: ethyl acetate/hexane=1/5)