反应详情

3-Pyridinemethanol (0.080 g, 0.731 mmol), triphenylphosphine (0.192 g, 0.731 mmol) and diethylazodicarboxylate (0.127 g, 0.731 mmol) were added to a benzene solution of N-[5-(3,4,5,6-tetramethoxy-2-methylbenzyl)-2-hydroxybenzoyl]morpholine (0.210 g, 0.487 mmol) and the solution was stirred at room temperature for 12 hours. The reaction solution was poured into an aqueous 2N sodium hydroxide solution (15 ml) and then extracted with methylene chloride. The extract was washed with water and then dried, and the solvent was removed by distillation. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=1.5:8.5) to obtain the titled compound (0.195 g, 0.374 mmol, 77%).

1. extractionextracted with methylene chloride
2. washThe extract was washed with water
3. customdried
4. customthe solvent was removed by distillation
5. customThe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=1.5:8.5)