反应详情

To 2-(acetamido)pyridine-4-carboxylic acid (25 g, 139 mmol) was added a saturated solution of anhydrous hydrogen chloride in methanol (600 mL). The cloudy suspension was stirred for 16 h at RT and refluxed for 24 h. The resulting solution was concentrated, dissolved in chloroform, washed with saturated sodium bicarbonate, brine, dried (magnesium sulfate) and concentrated to give the title compound as a white solid (17.86 g, 84%). TLC Rf 0.55 (5% methanol/chloroform); 1H NMR (CDCl3) δ3.96 (3H, s), 4.80 (2H, s),7.12 (1H, J=5 Hz, d), 7.19 (1H, s), 8.10 (1H, d, J=5 Hz).

1. temperaturerefluxed for 24 h
2. concentrationThe resulting solution was concentrated
3. dissolutiondissolved in chloroform
4. washwashed with saturated sodium bicarbonate, brine
5. dry with materialdried (magnesium sulfate)
6. concentrationconcentrated