反应详情

0.5 g of 5,5-diphenylimidazolidine-2,4-dione was dissolved in tetrahydrofuran (5 mL), and sodium hydride (60%, in oil) (87 mg) was added at 0° C. under ice-cooling. After stirred for 30 minutes, 2-naphthoyl chloride (415 mg) was added at 0° C., followed by stirring at room temperature for 2.5 hours. After water was carefully added, ethyl acetate (200 mL) was added, and the layers were separated. The resulting organic layer was washed with a saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was distilled off. Further purification by silica gel chromatography (hexane:ethyl acetate=3:1) afforded white crystals. The resulting fraction was recrystallized from isopropyl ether (IPE) to obtain 441 mg of white crystals.

1. temperaturecooling
2. stirringby stirring at room temperature for 2.5 hours
3. customthe layers were separated
4. washThe resulting organic layer was washed with a saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off
7. customFurther purification by silica gel chromatography (hexane:ethyl acetate=3:1)
8. customafforded white crystals
9. customThe resulting fraction was recrystallized from isopropyl ether (IPE)