反应详情

A solution of ethyl 1,4-dioxaspiro[4,5]decane-8-acetate (50.0 g) in 50 mL of 4.8N sodium hydroxide solution and 400 mL of ethanol is refluxed under nitrogen for 2 hours. The mixture is concentrated in vacuo to remove the ethanol. The residue is acidified with a saturated sodium biphosphate solution and the mixture is extracted with ethyl acetate (2×300 mL). The organic extract is dried over magnesium sulfate, and evaporated in vacuo to give an oily solid which is triturated with hexane and filtered to give 38.25 g of the title compound as a white solid; mp 110°-113° C.

1. concentrationThe mixture is concentrated in vacuo
2. customto remove the ethanol
3. extractionthe mixture is extracted with ethyl acetate (2×300 mL)
4. extractionThe organic extract
5. dry with materialis dried over magnesium sulfate
6. customevaporated in vacuo
7. customto give an oily solid which
8. customis triturated with hexane
9. filtrationfiltered