反应详情

温度

80 °C

A suspension of N-(4-((2-(cyclopropanecarboxamido)pyridin-4-yl)oxy)-2,5-difluorophenyl)-4-ethoxy-1-(4-fluorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide (0.029 g, 0.051 mmol) in MeCN (0.5 mL) was heated to 80° C., treated with methanesulfonic acid (3.34 μl, 0.051 mmol), then cooled to RT and stirred overnight. Ether was added drop wise until solids precipitated. The mixture was stirred for several hours. The solids were collected by filtration, rinsed with ether and dried under vacuum to afford N-(4-((2-(cyclopropanecarboxamido)pyridin-4-yl)oxy)-2,5-difluorophenyl)-4-ethoxy-1-(4-fluorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxamide methanesulfonate (15 mg, 44% yield) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 11.22 (s, 1H), 10.99 (s, 1H), 8.33 (dd, J=12.6, 7.2 Hz, 1H), 8.20 (d, J=5.8 Hz, 1H), 7.92 (d, J=7.8 Hz, 1H), 7.63-7.45 (m, 4H), 7.36 (m, 2H), 6.79 (d, J=5.7 Hz, 1H), 6.55 (d, J=7.9 Hz, 1H), 4.28 (q, J=7.0 Hz, 2H), 2.29 (s, 3H), 1.93 (m, 1H), 1.33 (t, J=7.0 Hz, 3H), 0.77 (m, 4H); MS (ESI) m/z: 565.2 (M+H+).

1. temperaturecooled to RT
2. customprecipitated
3. stirringThe mixture was stirred for several hours
4. filtrationThe solids were collected by filtration
5. washrinsed with ether
6. customdried under vacuum