反应详情

A mixture containing 8.4 g of 4-methylene-2-oxo-3-phenyl-1-oxa-3,8-diazaspiro[4,5]decane, 18.4 g of 4,4-bis(4-fluorophenyl)-3-butenyl chloride, 0.3 g of potassium iodide, 9.2 g of anhydrous potassium carbonate and 81 ml of methyl isobutyl ketone is mildly refluxed under argon while stirring for 12 hours. After cooling down and filtering off the inorganic salts, the precipitate is washed with methyl isobutyl ketone, the filtrate is washed with water to neutral, dried over anhydrous magnesium sulfate, then the solvent is evaporated under reduced pressure. After triturating the evaporation residue with n-hexane, the precipitate is filtered and recrystallized from ethanol to give the title compound in 83.5% yield, m.p.: 136.5°-137.5° C.

1. temperatureis mildly refluxed under argon
2. temperatureAfter cooling down
3. filtrationfiltering off the inorganic salts
4. washthe precipitate is washed with methyl isobutyl ketone
5. washthe filtrate is washed with water to neutral,
6. dry with materialdried over anhydrous magnesium sulfate
7. customthe solvent is evaporated under reduced pressure
8. customAfter triturating the evaporation residue with n-hexane
9. filtrationthe precipitate is filtered
10. customrecrystallized from ethanol