反应详情

温度

60 °C

To a solution of Example 1D (30 mg, 0.14 mmol) in N,N-dimethylformamide (1 mL) was added potassium carbonate (57 mg, 0.41 mmol) and bromoethane (10.3 μl, 0.14 mmol). The reaction was warmed to 60° C. for 14 hours. Excess potassium carbonate was filtered off. The solution was passed through a PS-isocyanate cartridge (Silicycle, 2 g) to trap leftover starting material. The solution was concentrated and purified by preparative HPLC with a gradient of acetonitrile and 0.1% trifluoroacetic acid in water to afford the title compound. 1H NMR (500 MHz, DMSO-d6/D2O) δ ppm 7.19-7.24 (m, 1 H), 7.14-7.18 (m, 1 H), 7.09-7.13 (m, 1 H), 7.01 (dd, J=7.78, 1.37 Hz, 1 H), 3.52-3.64 (m, 3 H), 3.32-3.39 (m, 2 H), 3.19-3.27 (m, 2 H), 2.97-3.10 (m, 2 H), 2.66 (dd, J=13.73, 7.02 Hz, 1 H), 2.09 (d, J=13.12 Hz, 1 H), 1.27 (t, J=7.32 Hz, 3 H); MS (ESI) m/z 246.0 (M+H)+.

1. filtrationExcess potassium carbonate was filtered off
2. customThe solution was passed through a PS-isocyanate cartridge (Silicycle, 2 g) to trap
3. concentrationThe solution was concentrated
4. custompurified by preparative HPLC with a gradient of acetonitrile and 0.1% trifluoroacetic acid in water