反应详情

380 mg of 1-{4-[(5-nitro-2-pyridinyl)oxy]phenyl}-1-ethanone was dissolved in 5 ml of benzene and, after adding 98 μl of ethylene glycol and 3 mg of (±)-10-camphorsulfonic acid, the mixture was heated at reflux. After 3 hours, the reaction solution was extracted with ethyl acetate. The organic layer was washed in turn with a saturated sodium hydrogencarbonate solution and a saturated sodium chloride solution, dried over magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (eluent: ethyl acetate/n-hexane (1:4)) to obtain the titled compound (280 mg).

1. temperaturethe mixture was heated
2. temperatureat reflux
3. extractionthe reaction solution was extracted with ethyl acetate
4. washThe organic layer was washed in turn with a saturated sodium hydrogencarbonate solution
5. dry with materiala saturated sodium chloride solution, dried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue was purified by silica gel chromatography (eluent: ethyl acetate/n-hexane (1:4))