反应详情

温度

70 °C

A mixture of 4-bromo-6-fluoro-2-methylisoquinolin-1-one (500.00 mg, 1.95 mmol), 2-[2-(cyclopropylmethoxy)-5-ethylsulfonylphenyl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (1.07 g, 2.92 mmol), K3PO4 (1.24 g, 5.85 mmol) and Pd(dppf)Cl2 (0.1 g, cat.) in dioxane/H2O (30 mL/4 mL) was stirred at 70° C. for 12 hrs under Ar. The mixture was concentrated and the residue purified by column chromatography (PE:EA=1:1) to give a pink solid. The pink solid was further purified by column chromatography (DCM:EA=4:1) to afford the title compound (0.13 g, 16%) as a light yellow solid. 1H NMR (CDCl3, 400 MHz) δ 8.54 (brs, 1H), 7.96 (dd, J1=8.8 Hz, J2=2.4 Hz, 1H), 7.81 (d, J=2.0 Hz, 1H), 7.22-7.20 (m, 1H), 7.15-7.13 (m, 1H), 7.1 (d, J=8.8 Hz, 1H), 6.78 (dd, J1=10.4 Hz, J2=2.4 Hz, 1H), 3.90 (t, J=7.6 Hz, 2H), 3.68 (s, 3H), 3.15 (q, J=7.6 Hz, 2H), 1.33 (t, J=7.6 Hz, 3H), 1.06-1.02 (m, 1H), 0.50-0.43 (m, 2H), 0.15-0.14 (m, 2H). LCMS (M+H)+=416.0 (M+1)+

1. concentrationThe mixture was concentrated
2. customthe residue purified by column chromatography (PE:EA=1:1)
3. customto give a pink solid
4. customThe pink solid was further purified by column chromatography (DCM:EA=4:1)