反应详情

温度

140 °C

Potassium trifluoro(prop-1-en-2-yl)borate (53.3 mg, 0.360 mmol), N-(5-bromo-3-methoxypyridin-2-yl)-4-fluorobenzenesulfonamide (130 mg, 0.360 mmol), caesium carbonate (352 mg, 1.080 mmol), palladium(II) chloride (1.276 mg, 7.20 μmol) and triphenylphosphine (5.66 mg, 0.022 mmol) were added to a microwave vial and suspended in tetrahydrofuran (THF) (2 mL) and water (0.2 mL). The reaction vessel was sealed and heated by microwaves to 140° C. for 30 minutes. After cooling, the mixture was diluted with dichloromethane (DCM) (5 mL) and water (5 mL), then passed through a celite column. The aqueous phase was washed with further DCM (5 mL) then the organics separated using a hydrophobic frit and concentrated in vacuo to give the crude product. This was purified by flash silica (Si) chromatography (0-50% ethyl acetate-cyclohexane gradient) to give the title product (75 mg). LCMS (2 min, formic) Rt 1.0 min, m/z (ES+) 323 (M+H).

1. customThe reaction vessel was sealed
2. temperatureAfter cooling
3. washThe aqueous phase was washed with further DCM (5 mL)
4. customthe organics separated
5. concentrationconcentrated in vacuo
6. customto give the crude product
7. customThis was purified by flash silica (Si) chromatography (0-50% ethyl acetate-cyclohexane gradient)