反应详情

To a mixture of (E)-3-methoxy-6-((2,4,6-trimethoxystyrylsulfonyl)methyl)pyridin-2-amine (333 mg, 0.84 mmol) in dry pyridine (20 mL) cooling on an ice bath methanesulfonyl chloride (0.3 mL, 2 mmol) was added dropwise. The mixture was stirred at room temperature for 20 hours. After evaporated to dryness, the residue was purified by silica gel chromatography, eluting with PE/EtOAc (1:1 v/v) to afford 20 mg of the title compound as white powder. 1H-NMR (DMSO-d6): δ 3.26 (s, 3H, OCH3), 3.82 (s, 3H, CH3), 3.85 (s, 9H, 3×OCH3), 4.45 (s, 2H, CH2), 6.30 (s, 2H, Ph-H), 7.14 (d, 1H, J=15.6 Hz, CH), 7.15 (d, 1H, J=8.8 Hz, Py-H), 7.41 (d, 1H, J=8.4 Hz, Py-H), 7.56 (d, 1H, J=15.6 Hz, CH), 9.73 (s, 1H, NH).

1. additionwas added dropwise
2. customAfter evaporated to dryness
3. customthe residue was purified by silica gel chromatography
4. washeluting with PE/EtOAc (1:1 v/v)