反应详情

A 0.3 g quantity of sulfuryl chloride was added to 1.2 g of 3-(2,6-dichloro-4-trifluoromethylphenyl)-1-methyl-5-methylsulfenylpyrazole (compound 1) in 5 ml of anhydrous carbon tetrachloride at room temperature, followed by stirring at room temperature for 2 hours. The reaction mixture was poured into cold water, and the resulting mixture was extracted with methylene chloride. The organic layer was washed with 10% aqueous sodium hydrogen carbonate solution and with brine, and dried over anhydrous 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: ether/hexane=1/5), giving 1.0 g of the desired compound in the form of white crystals (yield 83.3%).

1. extractionthe resulting mixture was extracted with methylene chloride
2. washThe organic layer was washed with 10% aqueous sodium hydrogen carbonate solution and with brine
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationThe solvent was distilled off under reduced pressure
5. customto obtain a residue, which
6. customwas then purified by column chromatography on silica gel (eluent: ether/hexane=1/5)