反应详情

To an aqueous solution (2.0 mL) of (E)-5-[1,3]dioxolan-2-yl-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzylidene]valeric acid ethyl ester (480 mg), acetic acid (1.0 mL) and trifluoroacetic acid (1.0 mL) were added one by one, and the reaction solution was agitated at room temperature for 2.5 hours. A saturated sodium bicarbonate water and ethyl acetate were added to the reaction solution after confirming disappearance of the starting materials, and the organic layer was partitioned. After the obtained organic layer was washed with a saturated saline solution, it was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel chromatography (elution solvent:ethyl acetate→ethyl acetate:ethanol=10:1), and 400 mg of the title compound was obtained. The physical properties of the compound are as follows.

1. customthe organic layer was partitioned
2. washAfter the obtained organic layer was washed with a saturated saline solution, it
3. dry with materialwas dried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by silica gel chromatography (elution solvent:ethyl acetate→ethyl acetate:ethanol=10:1)