Phosphorus tribromide → 4-bromomethyl-5-chloro-3-difluoromethyl-1-methyl-1H-pyrazole

Temperature

-10 °C

A solution of 2.0 g (10.0 mmoles) of (5-chloro-3-difluoromethyl-1-methyl-1H-pyrazol-4-yl)-methanol dissolved in 50 ml of diethyl ether was cooled to −10° C. Thereto was added 1.0 g (3.5 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature overnight to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into ice water, followed by extraction with diethyl ether. 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 2.6 g (yield: 100.0%) of 4-bromomethyl-5-chloro-3-difluoromethyl-1-methyl-1H-pyrazole.

1. customto give rise
2. customto a reaction
3. customAfter the completion of the reaction
4. extractionfollowed by extraction with diethyl ether
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

ORD record

ord-076e16d4e4bb480aad9662ed6961b103

Source dataset

uspto-grants-2007_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07238689B2