反应详情

To a solution of 5-bromomethyl-2-methoxy-3-nitropyridine (4.92 g, 0.02 mol) in methanol (50 mL), mercaptomethyl acetate (2.7 mL, 0.03 mol) and sodium carbonate (2.12 g, 0.02 mol) were added at room temperature and stirred for 1 h. After evaporated to dryness, the mixture was dissolved in ethyl acetate (200 mL), filtered and concentrated under reduced pressure. Recrystallisation from EtOH (50 mL) gave the pure product as a pale green solid (3.99 g, 73%). M.p. 57-60° C.; 1H-NMR (DMSO-d6): δ 3.32 (s, 2H, CH2), 3.59 (s, 3H, OCH3), 3.90 (s, 2H, CH2), 4.03 (s, 3H, OCH3), 8.42 (d, 1H, J=2.0 Hz, Py-H), 8.44 (d, 1H, J=2.0 Hz, Py-H); 13C-NMR (DMSO-d6): δ 31.62, 32.60, 52.54, 55, 17, 128.35, 133.77, 136.05, 152.14, 155.16, 170.74; HR-MS (ESI+) m/z: 273.0573 [M+H]+; C7H6N2O3 requires 272.0467.

1. customAfter evaporated to dryness
2. dissolutionthe mixture was dissolved in ethyl acetate (200 mL)
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customRecrystallisation from EtOH (50 mL)