反应详情

温度

-10 °C

A solution of 3.0 g (10.9 mmoles) of (5-chloro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol dissolved in 60 ml of diethyl ether was cooled to −10° C. Thereto was added 1.0 g (3.8 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature for 1 hour to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein, to obtain 3.6 g (yield: 95.8%) of 4-bromomethyl-5-chloro-1-phenyl-3-trifluoromethyl-1H-pyrazole as white crystals.

1. customto give rise
2. customto a reaction
3. customAfter the completion of the reaction
4. extractionfollowed by extraction with ethyl acetate
5. washThe resulting organic layer was washed with an aqueous sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationThe resulting solution was subjected to vacuum distillation
8. customto remove the solvent