反应详情

温度

55 °C

A mixture of 3-aminobenzamide (136 mg, 1.0 mmol), 7C (170 mg, 1.0 mmol) and glyoxylic acid monohydrate (92 mg, 1.0 mmol) in acetonitrile (5.0 mL) and DMF (1.2 mL) was heated at 55° C. for 2.0 h and then stirred at rt for 18 h. After removal of solvent, the crude was purified by silica gel column chromatography eluting with gradient methanol in methylene chloride to give 7D as a solid (190 mg, 60% yield). 1H NMR (400 MHz, Methanol-d4) δ ppm 3.85 (s, 3H) 5.11 (s, 1H) 6.79 (d, J=7.03 Hz, 1H) 7.04-7.15 (m, 5H) 7.27 (dd, J=8.35, 1.76 Hz, 1H); LC-MS 319 (M+H).

1. customAfter removal of solvent
2. customthe crude was purified by silica gel column chromatography
3. washeluting with gradient methanol in methylene chloride