反应详情

To a solution of 7,7-ethylenedioxy-5-azaspiro[2,4]heptane in acetonitrile (50 mL) was dropwise added 3,4,5-trifluoronitrobenzene (5.3 g, 31.6 mmol) and the reaction mixture was refluxed for 3 hours. After the reaction was terminated, the reaction mixture was cooled to room temperature and the solvent was removed therefrom by vacuum distillation. It was diluted with ethyl acetate and water, and the organic phase thus formed was dried over magnesium sulfate. The residue was filtered, concentrated in a vacuum, and purified through column chromatography (n-hexane/ethyl acetate=4:1) to afford the target compound (3.5 g, yield 66%).

1. temperaturethe reaction mixture was refluxed for 3 hours
2. customAfter the reaction was terminated
3. customthe solvent was removed
4. distillationby vacuum distillation
5. additionIt was diluted with ethyl acetate and water
6. customthe organic phase thus formed
7. dry with materialwas dried over magnesium sulfate
8. filtrationThe residue was filtered
9. concentrationconcentrated in a vacuum
10. custompurified through column chromatography (n-hexane/ethyl acetate=4:1)