反应详情

Pentabromophenol (1.0 g, 2.05 mmol) and AlCl3 (4.1 g, 30.75 mmol) were mixed in toluene (20 mL) and heated at reflux temperature under a nitrogen atmosphere overnight. The reaction mixture was cooled, cautiously added to ice, filtered and the filtrate was extracted with EtOAc (3×50 mL). The organics were dried (Na2SO4) and concentrated in vacuo. The residue obtained was purified by chromatography on silica gel with EtOAc:heptane (1:4, v/v) as eluent to afford the title compound as a white solid (230 mg, 0.91 mmol, 45%).

1. temperatureheated
2. temperatureat reflux temperature under a nitrogen atmosphere overnight
3. temperatureThe reaction mixture was cooled
4. additioncautiously added to ice
5. filtrationfiltered
6. extractionthe filtrate was extracted with EtOAc (3×50 mL)
7. dry with materialThe organics were dried (Na2SO4)
8. concentrationconcentrated in vacuo
9. customThe residue obtained
10. customwas purified by chromatography on silica gel with EtOAc:heptane (1:4, v/v) as eluent