反应详情

ethyl 4-acetyl-benzoate (9.61 g, a product of the firm Wako Pure Chemical Ind.) was dissolved in toluene (200 ml) under an argon atmosphere whereto ethylene glycol (20 ml) and p-toluenesulfonic acid hydrate (200 mg) were added, whereupon the mixture was refluxed with heating for 24 hours while dehydrating on a Dean-Stark apparatus. After cooling down to room temerature, the toluene layer was washed with water (100 ml×twice) and with saturated aqueous sodium chloride solution (100 ml) succeedingly, followed by drying and concentrating to dryness under reduced pressure, whereby the above-identified compound was obtained (12.76 g).

1. additionwere added, whereupon the mixture
2. temperaturewas refluxed
3. temperaturewith heating for 24 hours
4. temperatureAfter cooling down to room temerature
5. washthe toluene layer was washed with water (100 ml×twice) and with saturated aqueous sodium chloride solution (100 ml) succeedingly
6. customby drying
7. concentrationconcentrating to dryness under reduced pressure, whereby the above-identified compound
8. customwas obtained (12.76 g)