反应详情

温度

100 °C

To a solution of the title compound from Example 2 Step D (0.135 g, 0.514 mmol) and the title compound from Example 3 Step B (0.079 g, 0.428 mmol) in tetrahydrofuran (4.28 mL) were added palladium acetate (9.61 mg, 0.043 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl (0.035 g, 0.086 mmol), and potassium phosphate tribasic (0.273 g, 1.284 mmol). The resulting mixture was heated at 100° C. for 18 hours, then filtered with the aid of ethyl acetate and concentrated under reduced pressure. Purification by flash chromatography on silica gel (50% acetone in dichloromethane) provided the title compound: LCMS m/z 286.17 [M+H]+; 1H NMR (500 MHz, CDCl3) δ 8.83 (s, 1H), 8.75 (s, 1H), 8.26 (d, J=2.0 Hz, 1H), 7.85 (s, 1H), 7.63 (dd, J=9.8, 5.1 Hz, 1H), 7.16-7.12 (m, 1H), 2.64 (s, 3H), 2.28 (br s, 1H), 1.67 (s, 6H).

1. filtrationfiltered with the aid of ethyl acetate
2. concentrationconcentrated under reduced pressure
3. customPurification by flash chromatography on silica gel (50% acetone in dichloromethane)