Potassium Carbonate → HCID 89656289, Verbindung

Temperatur

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. for 16 hours. 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. The crude material was purified by flash chromatography (silica gel, 0-10% ethyl acetate/hexanes gradient) 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
9. customThe crude material was purified by flash chromatography (silica gel, 0-10% ethyl acetate/hexanes gradient)

ORD-Eintrag

ord-66633c66c80b47c39eb0ff25a40ec39f

Quelldatensatz

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09296741B2