反应详情

Methylene chloride (9.0 mL), pyridine (0.82 mL), and acetic anhydride (0.46 mL) were sequentially added to the obtained 2-hydroxy-5-(piperidin-1-yl)benzoic acid (0.90 g), followed by stirring at room temperature for 2 hours. The solvent was evaporated under reduced pressure, and a 10% aqueous solution of citric acid and ethyl acetate were added thereto. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, and the resulting mixture was washed with water and a saturated aqueous solution of sodium chloride sequentially, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and diisopropyl ether was added to the obtained residue. The solid substance was collected by filtration to obtain 0.55 g of 2-acetoxy-5-(piperidin-1-yl)benzoic acid as a light yellow solid.

1. customThe solvent was evaporated under reduced pressure
2. additiona 10% aqueous solution of citric acid and ethyl acetate were added
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted with ethyl acetate
5. washthe resulting mixture was washed with water
6. dry with materiala saturated aqueous solution of sodium chloride sequentially, and dried over anhydrous magnesium sulfate
7. customThe solvent was evaporated under reduced pressure, and diisopropyl ether
8. additionwas added to the obtained residue
9. filtrationThe solid substance was collected by filtration