反应详情

One liter flask equipped with a Dean-Stark condenser was charged-with 166.3 g (1.0 mol) of 2-methyl-2-adamantanol (supplied by Sigma-Aldrich Co.), 2.0 g (20 mmol) of sulfuric acid and 500 g of toluene. The content was heated to the solvent reflux temperature. While toluene and water produced through the reaction were collected as an azeotrope by the Dean-Stark condenser, the reaction mixture was refluxed for 2 hours. After completion of the reaction, the catalyst was removed by washing the reaction mixture with water and the obtained organic phase was concentrated to dryness to give 152.5 g of white solid 2-methyleneadamantane (purity: 99.0%, yield: 98.0%).

1. customOne liter flask equipped with a Dean-Stark condenser
2. temperatureThe content was heated to the solvent
3. temperaturereflux temperature
4. customwere collected as an azeotrope by the Dean-Stark condenser
5. temperaturethe reaction mixture was refluxed for 2 hours
6. customAfter completion of the reaction
7. customthe catalyst was removed
8. washby washing the reaction mixture with water
9. concentrationthe obtained organic phase was concentrated to dryness