Water → 3-(Bromomethyl)-4-(trifluoromethyl)pyridine

A solution of 0.6 g (3.4 mmoles) of (4-trifluoromethylpyridin-3-yl)-methanol dissolved in 50 ml of diethyl ether was cooed to −30° C. Thereto was added 1.4 g (5.2 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, followed by extraction with ethyl acetate. 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 vacuum distillation to remove the solvent contained therein, to obtain 0.61 g (yield: 75.3%) of 3-bromomethyl-4-trifluoromethylpyridine as a yellow oily substance.

1. customwas cooed to −30° C
2. customto give rise
3. customto a reaction
4. customAfter confirmation of the completion of the reaction
5. extractionfollowed by extraction with ethyl acetate
6. washThe resulting organic layer was washed with water
7. dry with materialan aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate
8. distillationThe resulting solution was subjected to vacuum distillation
9. customto remove the solvent

ORD record

ord-33ec21408bc942ac892ac95eb5f9dc2f

Source dataset

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07833939B2