反应详情

Dimethyl sulphate (30 ml) was added dropwise over 45 min to a stirred mixture of 5-fluoro-2-hydroxyacetophenone (32.43 g) and potassium carbonate (40.5 g) in acetone (500 ml) and the mixture was then heated under reflux for 8 hr. Concentrated ammonia solution was added and the inorganic solids removed by filtration. The solvent was removed under reduced pressure and the product was dissolved in ether and washed with water. After drying the ethereal solution (Na2SO4) the ether was removed under reduced pressure and the residue was distilled to give 5-fluoro-2-methoxyacetophenone (28.4 g); b.p. 58°-64 ° C./0.2 mm.

1. temperaturethe mixture was then heated
2. temperatureunder reflux for 8 hr
3. customthe inorganic solids removed by filtration
4. customThe solvent was removed under reduced pressure
5. dissolutionthe product was dissolved in ether
6. washwashed with water
7. dry with materialAfter drying the ethereal solution (Na2SO4) the ether
8. customwas removed under reduced pressure
9. distillationthe residue was distilled