反应详情

To a stirred suspension of 4-hydroxybenzaldehyde (0.500 g, 4.012 mmol) and anhydrous potassium carbonate (0.833 g, 6.019 mmol) in dry MeCN (15 ml) at room temperature was added 2-bromo-1-tert-butyldimethylsiloxyethane (83%, 1.730 g, 6.019 mmol), and the reaction mixture was heated under reflux for 20.5 h. Water (25 ml) was added and the reaction mixture was extracted with Et2O (4×25 ml). The combined organic extracts were washed with brine (50 ml), dried (Na2SO4), and the solvent was removed under reduced pressure to give a pale yellow oil that was purified by flash chromatography (3:1 Hexane/Et2O) to give the title compound (0.895 g, 79.5%) as a colourless oil.

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 20.5 h
3. extractionthe reaction mixture was extracted with Et2O (4×25 ml)
4. washThe combined organic extracts were washed with brine (50 ml)
5. dry with materialdried (Na2SO4)
6. customthe solvent was removed under reduced pressure
7. customto give a pale yellow oil that
8. customwas purified by flash chromatography (3:1 Hexane/Et2O)