反应详情

温度

70 °C

To a solution of 5-bromo-3-methoxy-1-methylpyridin-2-one (694 mg, 3.18 mmol), 2-(5-ethylsulfonyl-2-fluorophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (1 g, 3.18 mmol), Pd(dppf)Cl2 (233 mg, 318.00 umol) in dioxane (26 mL) and H2O (2.6 mL) was added K3PO4 (2.02 g, 9.54 mmol, 3.00 Eq). The reaction was stirred at 70° C. under N2 for 6 hrs. The mixture was concentrated and the residue was purified by silica gel column chromatography (PE/EA=3/1 to 1/2) to afford the title compound (0.9 g, 87%) as a brown solid. 1H NMR (CDCl3, 400 MHz) δ 7.93 (dd, J1=7.2 Hz, J2=2.0 Hz, 1H), 7.88-7.84 (m, 1H), 7.35 (dd, J1=10.0 Hz, J2=8.8 Hz, 1H), 7.23 (d, J=1.6 Hz, 1H), 6.83 (s, 1H), 3.89 (s, 3H), 3.67 (s, 3H), 3.16 (q, J=7.6 Hz, 2H), 1.33 (t, J=7.6 Hz, 3H). LCMS: 325.9 (M+H)+

1. concentrationThe mixture was concentrated
2. customthe residue was purified by silica gel column chromatography (PE/EA=3/1 to 1/2)