反应详情

A mixture of 4-(5-trifluoromethyl-2-pyridyloxy)phenol (25.6 g), N-[(±)-2-chloropropionyl]isoxazolidine (16.4 g) which was prepared as in Example 1, anhydrous potassium carbonate (15.2 g) and acetonitrile (300 ml) was heated under reflux with stirring for 5 hours. After cooling, the reaction mixture was filtered through a suction filter to remove solid matters and the filtrate was concentrated in vacuo. The residue was washed with the addition of water and benzene and the organic layer formed was separated and dried over anhydrous sodium sulfate. The removal of the solvent by a distillation in vacuo gave N-[(±)-2-[4-(5-trifluoromethyl-2-pyridyloxy)phenoxy]propionyl]isoxazolidine (35.5 g) as a pale yellow crystalline solid. Recrystallization from a mixture of n-hexane/ethyl acetate yielded a white crystalline solid. m.p. 83°-85° C.

1. temperaturewas heated
2. temperatureunder reflux
3. temperatureAfter cooling
4. filtrationthe reaction mixture was filtered through a suction
5. filtrationfilter
6. customto remove solid matters
7. concentrationthe filtrate was concentrated in vacuo
8. washThe residue was washed with the addition of water and benzene
9. customthe organic layer formed
10. customwas separated
11. dry with materialdried over anhydrous sodium sulfate
12. customThe removal of the solvent
13. distillationby a distillation in vacuo