反应详情

温度

100 °C

The nitrile 25B (3.2 g, 14.4 mmol), 4-trifluoromethylphenylboronic acid (3.01 g, 1 mol eq), palladium acetate (65 mg, 0.02 mol eq), cesium carbonate (9.38 g, 2 mol eq), and XPhos (265 mg, 0.04 mol eq) were mixed, placed under a nitrogen atmosphere and dioxane (12 mL) was added. The mixture was heated at 100° C. overnight. After cooling, the mixture was filtered through a celite pad, washed with dioxane (2×30 mL) and concentrated under reduced pressure. The residue was purified by flash chromatography (7/3 Petroleum ether/EtOAc) to afford 26B as yellow solid (1.33 g, 40% Yield). 1HNMR (DMSO, 400 MHz) δ 3.63 (m, 4H, J=1.9), 3.74 (m, 4H, J=2), 7.38 (s, 1H), 7.74 (s, 1H), 7.84 (d, 2H, J=8.1), 8.32 (d, 2H, J=8).

1. temperatureAfter cooling
2. filtrationthe mixture was filtered through a celite pad
3. washwashed with dioxane (2×30 mL)
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by flash chromatography (7/3 Petroleum ether/EtOAc)