Water → 5-Bromo-4-chloro-6-(trifluoromethyl)pyrimidine

24.3 g (100.0 mmoles) of 5-bromo-4-hydroxy-6-trifluoromethylpyrimidine was suspended in 18.5 g (120.0 mmoles) of phosphorus oxychloride. The suspension was stirred at 100° C. for 2 hours to give rise to a reaction. After confirmation of the completion of the reaction, the reaction mixture was gradually poured into water and extraction with chloroform 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 purified by silica gel column chromatography to obtain 21.5 g (yield: 82.4%) of 5-bromo-4-chloro-6-trifluoromethylpyrimidine.

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 in this order and then dried over anhydrous magnesium sulfate
6. distillationThe resulting solution was subjected to reduced pressure distillation
7. customto remove the solvent
8. customThe residue was purified by silica gel column chromatography

ORD-Eintrag

ord-1571258e7a394e5997e2b14e2e997dad

Quelldatensatz

uspto-grants-2011_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07875606B2