反应详情

A mixture consisting of 35 g of 4-nitrophenol, 35 g of chloroacetone, 35 g of potassium carbonate, 1 g of potassium iodide and 500 ml of acetone was heated at reflux with stirring for 3 hr. Reaction mixture was concentrated underd reduced pressure; the concentrate was extracted with ethyl acetate; the ethyl acetate layer was washed consecutively with 5% aqueous solution of sodium hydroxide, water and saturated saline; and dried with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure; the residue was dissolved in 300 ml of ethanol, added with 100 ml of n-hexane; and subsequently left standing overnight at room temperature. Yellow crystals thus isolated were filtered off, dried and yielded 43.5 g of 4-nitrophenoxyacetone.

1. temperaturewas heated
2. temperatureat reflux
3. customReaction mixture
4. concentrationwas concentrated underd reduced pressure
5. extractionthe concentrate was extracted with ethyl acetate
6. washthe ethyl acetate layer was washed consecutively with 5% aqueous solution of sodium hydroxide, water and saturated saline
7. dry with materialand dried with anhydrous sodium sulfate
8. distillationThe solvent was distilled off under reduced pressure
9. dissolutionthe residue was dissolved in 300 ml of ethanol
10. additionadded with 100 ml of n-hexane
11. waitand subsequently left
12. waitstanding overnight at room temperature
13. customYellow crystals thus isolated
14. filtrationwere filtered off
15. customdried