反应详情

温度

50 °C

To a solution of 5-chloro-6-isopropoxypyridin-3-ol (Preparation 35, 350 mg, 1.87 mmol) in dimethyl sulfoxide (2 mL) was added 3-bromo-4-fluorobenzonitrile (333 mg, 1.87 mmol) and potassium carbonate (386 mg, 2.80 mmol). The reaction was stirred at 50° C. for 4 hours and then partitioned between water (100 mL) and EtOAc. The aqueous phase was separated and extracted with EtOAc (2×25 mL). The combined organic extracts were dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to afford the title compound as a colourless oil which crystallised on standing (920 mg) and which was used without further purification in the next step.

1. custompartitioned between water (100 mL) and EtOAc
2. customThe aqueous phase was separated
3. extractionextracted with EtOAc (2×25 mL)
4. dry with materialThe combined organic extracts were dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo