反应详情

温度

25 °C

A mixture of 4-fluorophenoxyacetaldehyde diethyl acetal (30 g., 0.13 mole), acetone (150 ml.), water (150 ml.) and concentrated sulfuric acid (0.8 ml.) is stirred and heated at reflux for 16 hours. After cooling to 25° C., the reaction mixture is extracted with methylene chloride four times. The combined organic extract is washed with aqueous sodium bicarbonate, dried over magnesium sulfate, and filtered. Evaporation of the filtrate in vacuo leaves a residual oil which is distilled to provide the title compound as a colorless oil (19 g., 94%) bp0.05 70° C.; pmr (CCl4) δ4.37 (2H, d), 6.6-7.1 (4H, m) and 9.68 (H, t).

1. temperatureheated
2. temperatureat reflux for 16 hours
3. extractionthe reaction mixture is extracted with methylene chloride four times
4. extractionThe combined organic extract
5. washis washed with aqueous sodium bicarbonate
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. customEvaporation of the filtrate in vacuo
9. customleaves a residual oil which
10. distillationis distilled