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

77.5 g (945.0 mmoles) of anhydrous sodium acetate was added, at room temperature, to 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 50.3 g (315 mmoles) of bromine at 45° C. The resulting 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 vacuum distillation to remove the solvent contained therein. The residue was poured into water, followed by extraction with ethyl acetate. 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 vacuum 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.

1. customat 45° C
2. customto give rise
3. customto a reaction
4. customAfter confirmation of the completion of the reaction
5. distillationthe reaction mixture was subjected to vacuum distillation
6. customto remove the solvent
7. additionThe residue was poured into water
8. extractionfollowed by extraction with ethyl acetate
9. washThe resulting organic layer was washed with water
10. dry with materialan aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate
11. distillationThe resulting solution was subjected to vacuum distillation
12. customto remove the solvent
13. washThe residue was washed with n-hexane

ORDレコード

ord-039e291b8f8c4582b3193aa8c5be56ed

出典データセット

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07833939B2