反应详情

In 200 ml of ethanol was dissolved 30.0 g of 4-hydroxyacetophenone, and a solution of 11.3 g (1.28 eq.) of sodium hydroxide in 60 ml of water and 33.9 g (1.22 eq.) of dimethyl sulfate were added dropwise consecutively. After the reaction mixture was refluxed for 30 minutes', a solution of 2.8 g (0.32 eq.) of sodium hydroxide dissolved in 10 ml of water was added, followed by heating under for 3 hours' reflux. After the solvent was distilled off, water was added and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. Then, the solvent was distilled off. The resulting crystals were collected by filtration with hexane.

1. additionwas added
2. temperatureby heating under for 3 hours'
3. temperaturereflux
4. distillationAfter the solvent was distilled off
5. additionwater was added
6. extractionthe mixture was extracted with ethyl acetate
7. washThe organic layer was washed with water
8. dry with materiala saturated aqueous solution of sodium chloride, and dried
9. distillationThen, the solvent was distilled off
10. filtrationThe resulting crystals were collected by filtration with hexane