Potassium Carbonate → 2-Bromo-1-(2,4-difluorophenoxy)-4-(trifluoromethyl)benzene

温度

80 °C

A mixture of 3-bromo-4-fluorobenzotrifluoride (0.5 mL, 3.52 mmol), 2,4-difluorophenol (0.337 mL, 3.52 mmol), and potassium carbonate (0.486 g, 3.52 mmol) in dimethylformamide (7 mL) was heated at 80° C. overnight. The reaction mixture was cooled to ambient temperature and partitioned between ethyl acetate and water. The layers were separated, and the aqueous layer was extracted with ethyl acetate. The combined organics were washed with water and saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, filtered, and concentrated by rotary evaporation. The crude material was purified by flash chromatography (ethyl acetate/hexanes) to provide the title compound (1.0 g, 80% yield).

1. temperatureThe reaction mixture was cooled to ambient temperature
2. custompartitioned between ethyl acetate and water
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with ethyl acetate
5. washThe combined organics were washed with water and saturated aqueous sodium chloride
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated by rotary evaporation
9. customThe crude material was purified by flash chromatography (ethyl acetate/hexanes)

ORDレコード

ord-8058b1143cce49648c28259edfb111e8

出典データセット

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09050346B2