反应详情

4-Pyridinemethanol (0.232 g, 2.13 mmol), tri-n-butylphosphine (0.430 g, 2.13 mmol) and N,N,N′,N′-tetramethylazodicarboxamide (0.366 g, 2.13 mmol) were added to a benzene solution of methyl 5-(3,4,5,6-tetramethoxy-2-methylbenzyl)-2-hydroxybenzoate (0.500 g, 1.33 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 (hexand:ethyl acetate=2:3) to obtain the titled compound (0.610 g, 1.31 mmol, 98%).

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 (hexand:ethyl acetate=2:3)