反应详情

温度

100 °C

To ethyl (E)-3-(6-amino-4-methylpyridin-3-yl)acrylate (1.50 g, 7.3 mmole) was added HOAc (15 mL) and conc. HCl (15 mL). The solution was stirred at 100° C. for 10 hr, cooled to RT, and concentrated to dryness. Trituration with Et2O, filtration and drying under vacuum gave the title compound (1.65 g, quantitative) as a white solid: LCMS (ES) m/e 179.2 (M+H)+; 1H NMR (400 MHz, DMSO-d6) δ 8.37 (s,1H), 8.28 (br s, 3H), 7.51 (d, I=16.0 Hz,1H), 6.86 (s,1H), 6.46 (d, J=16.0 Hz,1H), 2.41 (s, 3H).

1. temperaturecooled to RT
2. concentrationconcentrated to dryness
3. filtrationTrituration with Et2O, filtration
4. customdrying under vacuum