反应详情

温度

120 °C

To a pressure vessel, a mixture of 6-chloro-2-methyl-3-nitro-pyridin-4-ylamine (0.75 g, 4.00 mmol) and morpholine (1.40 mL, 16.0 mmol) in absolute ethanol (16 mL) was stirred at 120° C. for 3 days. Absolute ethanol was evaporated in vacuo and the crude product was dissolved in a mixture of THF:EtOAc and this then subjected on top of a silica gel pad. Elution with EtOAc gave, after evaporation, the title compound as a yellow solid (0.89 g, 93%): IR (KBr, cm−1) 3460, 3330, 1627, 1597, 1553, 1233, 1113; 1H NMR (400 MHz, DMSO) δ 7.13 (s, 2H), 5.89 (s, 1H), 3.66-3.63 (m, 4H), 3.46-3.44 (m, 4H), 2.50 (s, 3H); LCMS (+ESI, M+H+) m/z 239; HPLC: 99% (220 nm).

1. customAbsolute ethanol was evaporated in vacuo
2. dissolutionthe crude product was dissolved in a mixture of THF
3. washElution with EtOAc
4. customgave
5. customafter evaporation