反应详情

温度

70 °C

To a solution of compound (iii) (4.7 mg, 0.0084 mmol) and isobutylamine (0.1 mL) in 1,4-dioxane (0.3 mL) was heated to 40° C. and stirred for 45 min. More isobutylamine (100 μL) was added and the mixture was heated at 70° C. for 1.5 h. The mixture was cooled to RT and concentrated under reduced pressure. The residue was purified by preparative LCMS (5-30-50-100% acetonitrile in 0.1% aqueous formic acid) to give Compound (110) as a white solid. ESI-MS m/z calculated for [M+H]+: 485.2; found: 485.2; 1H NMR (400 MHz, CDCl3) δ 8.11 (d, J=1.9 Hz, 1H), 7.86 (dd, J=9.3, 2.1 Hz, 1H), 7.68 (s, 1H), 7.32 (s, 1H), 6.82 (brs, 1H), 6.69 (d, J=9.3 Hz, 1H), 6.17 (brs, 1H), 3.88-3.71 (m, 2H), 3.24-3.13 (m, 2H), 3.08 (s, 3H), 3.03 (d, J=4.9 Hz, 3H), 2.39 (ddd, J=13.9, 8.4, 5.5 Hz, 1H), 2.04-1.89 (m, 1H), 1.23 (t, J=7.1 Hz, 3H), 1.11-0.97 (m, 9H), 0.66-0.45 (m, 1H).

1. temperatureThe mixture was cooled to RT
2. concentrationconcentrated under reduced pressure
3. customThe residue was purified by preparative LCMS (5-30-50-100% acetonitrile in 0.1% aqueous formic acid)