反应详情

温度

60 °C

1,4-Dioxane (10 ml) and 3 M aq K3PO4 (1.12 mL, 3.3 mmol) was added to a flask containing [4-(methylthio)phenyl]boronic acid (0.283 g, 1.68 mmol), Pd(dppf)Cl2 (82 mg, 0.112 mmol) and ethyl (2R)-4-(5-fluoro-4-iodo-2-oxopyridin-1(2H)-yl)-2-methyl-2-(methylsulfonyl)butanoate, T2, (500 mg, 1.12 mmol) that was previously flushed with nitrogen. The mixture was heated to 60° C. and stirred at this temperature for 1 h. The reaction mixture was diluted with EtOAc and washed with water. The organics were dried (MgSO4), filtered, and concentrated. The crude product was purified via flash chromatography on a 40 g silica column and an eluent of EtOAc in n-heptane (0-100%) to afford the title compound as a gum (492 mg, 99%). MS (LCMS) m/z 442.1 (M+1). 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 1.17-1.27 (m, 3H) 1.74 (s, 3H) 2.38-2.61 (m, 5H) 3.09 (s, 3H) 3.88-4.02 (m, 1H) 4.17-4.32 (m, 3H) 6.57 (d, J=7.61 Hz, 1H) 7.21-7.34 (m, 3H) 7.37-7.48 (m, 2H).

1. customwas previously flushed with nitrogen
2. additionThe reaction mixture was diluted with EtOAc
3. washwashed with water
4. dry with materialThe organics were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product was purified via flash chromatography on a 40 g silica column