反应详情

After p-toluenesulfonic acid monohydrate (0.716 g, 3.77 mmol) was added to a solution of methyl (4′-{[2-(dimethoxymethyl)-3-(methoxymethoxy)-4-(trifluoromethyl)benzyl]oxy}-1,1′-biphenyl-3-yl)acetate (1.83 g, 3.43 mmol) obtained in Example (8-2) in acetone (20 ml), the mixture was stirred at room temperature for 6 hours. After the reaction mixture was poured into water and the mixture was extracted with ethyl acetate (twice), the organic layer was successively washed with water and a saturated aqueous NaCl solution and dried with anhydrous sodium sulfate. The solvent was removed under reduced pressure to give a residue. The obtained residue was purified by silica gel column chromatography (eluting solvent: n-hexane/ethyl acetate=80/20-70/30) to give methyl (4′-{[2-formyl-3-hydroxy-4-(trifluoromethyl)benzyl]oxy}-1,1′-biphenyl-3-yl)acetate (1.26 g, yield: 83%).

1. extractionthe mixture was extracted with ethyl acetate (twice), the organic layer
2. washwas successively washed with water
3. dry with materiala saturated aqueous NaCl solution and dried with anhydrous sodium sulfate
4. customThe solvent was removed under reduced pressure
5. customto give a residue
6. customThe obtained residue was purified by silica gel column chromatography (eluting solvent: n-hexane/ethyl acetate=80/20-70/30)