反应详情

To a solution of (2,6-dimethyl-4′-trifluoromethyl-biphenyl-4-yl)-methanol (2.22 g, 7.9 mmol) in THF (30 ml) is added PBr3 (3.22 g, 11.9 mmol) in THF (5 ml) and the reaction is allowed to stir at room temperature for about 2 h. The reaction is cooled to 0° C. and ice water is added slowly. The mixture is extracted with ethyl acetate, dried over MgSO4, and concentrated. The resulting residue is purified by silica gel column chromatography, eluting with EtOAc/hexanes to afford 2.2 g of the titled compound as a white solid. 1H-NMR.

1. temperatureThe reaction is cooled to 0° C.
2. extractionThe mixture is extracted with ethyl acetate
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customThe resulting residue is purified by silica gel column chromatography
6. washeluting with EtOAc/hexanes