反应详情

A solution of 2-((6-methoxy-5-nitropyridin-3-yl)methylsulfonyl)acetate (1.83 g, 6 mmol) and sodium carbonate (1.8 g, 15 mmol) in a mixture of water (10 mL) and methanol (10 mL) was stirred at room temperature for 4 hours. After evaporated to dryness, the residue was acidized by dropwise addition of 1N aq. HCl. White solid was precipitated gradually as pH was brought to 2 and filtrated to give the pure product (1.72 g, 98.7%). M.p. 183-186° C.; 1H-NMR (DMSO-d6): δ 4.06 (s, 3H, OCH3), 4.13 (s, 2H, CH2), 4.79 (s, 2H, CH2), 8.48 (d, 1H J=2.0 Hz, Py-H), 8.50 (d, 1H, J=2.0 Hz, Py-H); 13C-NMR (DMSO-d6): δ 55.07, 55.41, 57.15, 118.45, 133.64, 137.96, 154.26, 156.23, 164.88; HR-MS (ESI+) m/z: 289.0064 [M+H]+; C9H10N2O7S requires 290.0209

1. customAfter evaporated to dryness
2. additionthe residue was acidized by dropwise addition of 1N aq. HCl
3. customWhite solid was precipitated gradually as pH
4. filtrationfiltrated