反应详情

2 g of o-hydroxyacetophenone, 2.85 g of 4-nitrophenoxyacetone, 2 g of pyrrolidine and 280 mg of p-toluenesufonic acid monohydrate were dissolved in 10 ml of toluene, and the mixture was heated under reflux for 3 hours in apparatus equipped with a water separator. At the end of this time, the reaction mixture was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure. The residue was subjected to silica gel column chromatography eluted with a 3:1 by volume mixture of benzene and ethyl acetate, to afford 2.5 g of the title compound as a pale yellow oily substance.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 3 hours in apparatus
3. washAt the end of this time, the reaction mixture was washed with a saturated aqueous solution of sodium chloride
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationThe solvent was then distilled off under reduced pressure
6. washeluted with a 3:1 by volume mixture of benzene and ethyl acetate