反应详情

30.1 g of 8-(4-Fluoro-phenyl)-1,4-dioxa-spiro[4.5]decane-8-carbonitrile (74) were dissolved in 91 mL of ethylene glycol. 19.4 g of powdered potassium hydroxide were added and the mixture was heated to reflux until conversion was complete. The mixture was allowed to cool down to room temperature and poured into 300 mL of water. The pH was adjusted to 4 by addition of 2N HCl and the aqueous layer was extracted With ethyl acetate. The organic layer was extracted with brine, dried over magnesium sulfate and evaporated to dryness to give 29.85 g of the desired product. Rt=1.81 min (Method B). Detected mass: 281.2 (M+H+).

1. temperaturethe mixture was heated
2. temperatureto reflux until conversion
3. extractionthe aqueous layer was extracted With ethyl acetate
4. extractionThe organic layer was extracted with brine
5. dry with materialdried over magnesium sulfate
6. customevaporated to dryness