反应详情

温度

50 °C

Zirconiumtetrachloride (11.7 g, 50 mmol) in DCM (130 ml), tert-butylmethylether (4.44 g, 50 mmol), and 3-fluorophenol (5.6 g, 50 mmol) were mixed at room temperature and the reaction mixture was stirred for 2 hours at 50° C. The reaction was quenched with water and the whole was extracted with ethylacetate and dried over magnesium sulfate. After filtration, evaporation gave a crude residue, which was purified by silica gel column chromatography, eluting with gradually from hexane only to hexane/ethylacetate (9:1), to afford 4.25 g (51% yield) of the title compound as white solids.

1. customThe reaction was quenched with water
2. extractionthe whole was extracted with ethylacetate
3. dry with materialdried over magnesium sulfate
4. filtrationAfter filtration, evaporation
5. customgave a crude residue, which
6. customwas purified by silica gel column chromatography
7. washeluting with gradually from hexane only to hexane/ethylacetate (9:1)