Methanol → 5-Bromomethyl-4-ethoxy-6-trifluoromethylpyrimidine

Temperature

0 °C

A solution of 3.77 g (17.0 mmoles) of (4-ethoxy-6-trifluoromethylpyrimidine-5-yl)-methanol dissolved in 50 ml of diethyl ether was cooled to 0° C. Thereto was added 2.0 g (7.2 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature for 1 hour. The resulting salt was dissolved using methanol. The resulting mixture was stirred for 1 hour to give rise to a reaction. The reaction mixture was poured into 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 crude 5-bromomethyl-4-ethoxy-6-trifluoromethylpyrimidine.

1. dissolutionThe resulting salt was dissolved
2. stirringThe resulting mixture was stirred for 1 hour
3. customto give rise
4. customto a reaction
5. extractionfollowed by extraction with diethyl ether
6. washThe resulting organic layer was washed with an aqueous sodium chloride solution
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationThe resulting solution was subjected to vacuum distillation
9. customto remove the solvent

ORD record

ord-194d318e65b24b42b26abc0f6bd5f83e

Source dataset

uspto-grants-2007_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07238689B2