反应详情

温度

95 °C

3'-Chloromethyl-4'-hydroxyacetophenone (108 g.) was added to a mixture of anhydrous sodium acetate (54 g.) glacial acetic acid (500 ml.) and acetic anhydride (250 ml.). The mixture was heated at 95° C. for 4 hours, then concentrated by distilling under reduced pressure. The gummy residue was dissolved in water (500 ml.) and the aqueous solution was extracted with chloroform (3×300 ml.). The combined extracts were dried (MgSO4), filtered and evaporated to give a yellow oil. This was distilled under high vacuum to give 3'-acetoxymethyl-4'-acetoxyacetophenone as a colourless viscous liquid (108 g.), b.p. 143°-147° C. (0.3 mm.), which crystallised on cooling to give solid, m.p. 47°-48° C.

1. concentrationconcentrated
2. distillationby distilling under reduced pressure
3. dissolutionThe gummy residue was dissolved in water (500 ml.)
4. extractionthe aqueous solution was extracted with chloroform (3×300 ml.)
5. dry with materialThe combined extracts were dried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. customto give a yellow oil
9. distillationThis was distilled under high vacuum