Bromine → 5-bromo-6-(trifluoromethyl)-1H-pyrimidin-4-one

Participants

Reaction Steps

77.5 g (945.0 mmoles) of anhydrous sodium acetate was added, at room temperature, into a solution of 49.2 g (300.0 mmoles) of 4-hydroxy-6-trifluoromethylpyrimidine dissolved in 600 ml of acetic acid. Thereto was gradually added, at 45° C., 50.3 g (315 mmoles) of bromine. The mixture was stirred at the same temperature for 3 hours to give rise to a reaction. After confirmation of the completion of the reaction, the reaction mixture was subjected to reduced pressure distillation to remove the solvent contained therein. The residue was poured into water and extraction with ethyl acetate was conducted. The resulting organic layer was washed with water and an aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to reduced pressure distillation to remove the solvent contained therein. The residue was washed with n-hexane to obtain 38.9 g (yield: 53.4%) of 5-bromo-4-hydroxy-6-trifluoromethylpyrimidine.

Provenance & Evidence