反应详情

To a THF (10 ml) and methanol (5 ml) solution of the (8-methyl-1,4,7,9-tetraoxaspiro[4.5]dec-8-yl)methyl benzoate (1.92 g, 6.52 mmol) obtained in the step (5b), a 1N aqueous sodium hydroxide solution (10 ml, 10 mmol) was added and stirred at room temperature for one hour. The reaction mixture was extracted with dichloromethane (50 ml) four times, dried over anhydrous sodium sulfate, and then, concentrated. The obtained crude product was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate=1/1-0/1 gradient) and desired fractions were concentrated to obtain the title compound (1.12 g, 90.0% yield) as a white solid.

1. extractionThe reaction mixture was extracted with dichloromethane (50 ml) four times
2. dry with materialdried over anhydrous sodium sulfate
3. concentrationconcentrated
4. customThe obtained crude product
5. customwas purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate=1/1-0/1 gradient)
6. concentrationdesired fractions were concentrated