反应详情

温度

60 °C

(E)-ethyl 2-(2-methoxy-5-((2,4,6-trimethoxystyrylsulfonyl)methyl)pyridin-3-ylamino)acetate (20 mg, 0.04 mmol) was added to a solution of ammonia (5 mL 7N in methanol) and H2O (5 mL). The mixture was stirred at 60° C. for 4 h. After evaporated to dryness, the residue was purified by silica gel chromatography, eluting with PE/EtOAc (1:1, v/v) to afford pure product as a brown powder (9.2 mg, 26%). 1H-NMR (CDCl3): δ 3.80 (d, 2H, J=1.6 Hz, CH2), 3.87 (s, 6H, 2×OCH3), 3.87 (s, 3H, OCH3), 4.01 (s, 3H, OCH3), 4.16 (s, 2H, CH2), 5.43 (s, 1H, NH), 6.12 (s, 2H, Ph-H), 6.75 (d, 1H, J=2.0 Hz, Py-H), 7.09 (d, 1H, J=15.6 Hz, CH), 7.56 (d, 1H, J=2.0 Hz, Py-H), 7.81 (d, 1H, J=15.6 Hz, CH); HR-MS (ESI+) m/z 452.1560 [M+H]+ C20H25N3O7S requires 451.1413.

1. customAfter evaporated to dryness
2. customthe residue was purified by silica gel chromatography
3. washeluting with PE/EtOAc (1:1