Water → 4-bromomethyl-5-fluoro-1-methyl-3-trifluoromethyl-1H-pyrazole

Temperature

-30 °C

A solution of 35.4 g (178.7 mmoles) of 5-fluoro-1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboaldehyde dissolved in 500 ml of diethyl ether was cooled to −30° C. Thereto was added 54.0 g (199.5 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature for 12 hours to give rise to a reaction. After confirmation of the completion of the reaction, the reaction mixture was poured into water and extraction with diethyl ether was conducted. The resulting organic layer was washed with water and an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to reduced pressure distillation to remove the solvent contained therein, to obtain 31.4 g (yield: 80.8%) of 4-bromomethyl-5-fluoro-1-methyl-3-trifluoromethyl-1H-pyrazole.

1. customto give rise
2. customto a reaction
3. customAfter confirmation of the completion of the reaction
4. washThe resulting organic layer was washed with water
5. dry with materialan aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate
6. distillationThe resulting solution was subjected to reduced pressure distillation
7. customto remove the solvent

ORD record

ord-12b692ea47794715a90e3cfe712967db

Source dataset

uspto-grants-2011_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07875606B2