反应详情

5-Amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfinylpyrazole (0.97 g, 2.22 mmol) was dissolved in 10 ml of 1,4-dioxane and dimethylamine (50% aqueous solution) (1.20 ml, 11.4 mmol) was added, and then the mixture was stirred at room temperature for 5 days. After stirring, 20 ml of water and 20 ml of an aqueous saturated sodium chloride solution were added and the solution was extracted twice with 30 ml of ethyl acetate. The extract was dried over anhydrous magnesium sulfate and the solvent was distilled off to obtain a yellow amorphous. The amorphous was subjected to silica gel column chromatography [eluent: mixed solvent of ethyl acetate and methanol (volume ratio=4:1)] and a small amount of ether was added to crystallize the resulting amorphous. This resultant was filtered to obtain 0.29 g (0.60 mmol) of the title compound as a colorless crystal. Yield 27%.

1. stirringAfter stirring
2. extractionthe solution was extracted twice with 30 ml of ethyl acetate
3. dry with materialThe extract was dried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled off
5. customto obtain a yellow amorphous
6. customto crystallize the resulting amorphous
7. filtrationThis resultant was filtered