反应详情

To a solution of cyclohexanone (9.52 g, 97.0 mmol), a zinc powder (7.6 g, 116.4 mmol) and a small amount of iodine in THF (100 ml) was added dropwise ethyl bromoacetate (11.8 ml, 106.7 mmol) under a nitrogen atmosphere, and the mixture was heated under reflux for 5 hrs. 10% Sulfuric acid (100 ml) was carefully added under ice-cooling, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution, dried over anhydrous MgSO4, and concentrated under reduced pressure to give the title compound (17.2 g, 94%) as a colorless oil.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 5 hrs
3. temperaturecooling
4. extractionthe mixture was extracted with ethyl acetate
5. washThe extract was washed with saturated aqueous sodium hydrogen carbonate solution
6. dry with materialdried over anhydrous MgSO4
7. concentrationconcentrated under reduced pressure