反应详情

温度

70 °C

A mixture of the title compound from step 3 (100 mg, 0.31 mmol), 1,3-dimethyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-one (93 mg, 0.37 mmol), Pd(dppf)Cl2 (23 mg, 0.31 mmol) and K3PO4 (199 mg, 0.94 mmol) in dioxane/water (3 mL/0.5 mL) was N2 purged and heated at 70° C. for 12 h. Concentration under vacuum and silica gel chromatography (PE: EA=3:1˜0:1) followed by prep-HPLC gave the title compound (45 mg, 35.4%). 1H NMR (CDCl3, 400 MHz) δ 8.57 (s, 1H), 8.25 (s, 1H), 8.15 (s, 1H), 7.25-7.24 (m, 1H), 7.12-7.07 (m, 1H), 7.03 (t, J=8.0 Hz, 1H), 3.68 (s, 3H), 3.38 (s, 3H), 2.25 (s, 3H). LCMS: 407.9 (M+1)+

1. custompurged
2. concentrationConcentration under vacuum and silica gel chromatography (PE: EA=3:1˜0:1)