反应详情

温度

80 °C

A suspension of 4-ethyl-5-fluoro-2-methoxyphenol (1 g, 5.87 mmol), 3,4-difluorobenzonitrile (899 mg, 6.46 mmol) and potassium hydroxide (395 mg, 7.04 mmol) in anhydrous acetonitrile (35 mL) under argon was stirred at 80° C. overnight. The reaction mixture was concentrated under vacuum and diluted with ethyl acetate and a saturated aqueous solution of ammonium chloride. The aqueous layer was separated and extracted twice with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtrated and concentrated in vacuo to give a brown oil (1.6 g). The crude product was purified by flash chromatography on silica gel, using cyclohexane/ethyl acetate (9:1) as eluent. The title product was obtained as a colourless oil that crystallized slowly (1.42 g, 84%).

1. concentrationThe reaction mixture was concentrated under vacuum
2. additiondiluted with ethyl acetate
3. customThe aqueous layer was separated
4. extractionextracted twice with ethyl acetate
5. dry with materialThe combined organic phases were dried over sodium sulfate
6. filtrationfiltrated
7. concentrationconcentrated in vacuo