反应详情

3-Methyl-4-nitrobenzyl chloride (1.81 g), 3,5-bis(trifluoromethyl)-1H-pyrazole (2.0 g) and potassium carbonate (1.63 g) were stirred in DMF (20 ml) at 60° C. for 1 hour. After finishing the reaction, water (100 ml) was added thereto and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous solution of sodium chloride (100 ml) and dried with anhydrous sodium sulfate. After distilling off the solvent, the obtained residue was purified by silica gel column chromatography to obtain 1-(3-methyl-4-nitrobenzyl)-3,5-bis-(trifluoromethyl)-1H-pyrazole (3.3 g).

1. additionwas added
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with saturated aqueous solution of sodium chloride (100 ml)
4. dry with materialdried with anhydrous sodium sulfate
5. distillationAfter distilling off the solvent
6. customthe obtained residue was purified by silica gel column chromatography