反应详情

温度

-15 °C

To a solution of 80 g (0.349 mol) 2-bromomethylphenylacetic acid in 700 mL 1,4-dioxane in a 2 L heavy-walled flask was added 84 mL (1.571 mol) concentrated sulfuric acid at ambient temperature. The reaction mixture was chilled to −15° C., and 580 mL isobutylene was condensed directly into the reaction vessel. The sealed pressure flask was shaken mechanically at room temperature for 4 h (the pressure inside the flask rises to ca. 20 psi during this step). The mixture was carefully quenched by slowly pouring it into a 0-5° C. stirred mixture of 1.2 L tert-butyl methyl ether and 336 g (4.0 mol) solid sodium bicarbonate before slow dilution with 1.2 L ice-water. The separated organic phase was washed with 0.8 L brine, dried with sodium sulfate, filtered concentrated in vacuo to give an oil, which was used without further purification.

1. customcondensed directly into the reaction vessel
2. customThe mixture was carefully quenched
3. additionby slowly pouring it into a 0-5° C.
4. stirringstirred
5. washThe separated organic phase was washed with 0.8 L brine
6. dry with materialdried with sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customto give an oil, which
10. customwas used without further purification