反应详情

To (2′-hydroxymethyl-6-methoxy-4′-trifluoromethyl-biphenyl-3-yl)-acetic acid methyl ester (1.855 g, 5.23 mmol) in DME (19 mL) was added phosphorus tribromide (0.74 mL, 7.85 mmol), and the reaction was stirred at room temperature for 1.5 hours. The mixture was cooled to 0° C., and saturated aqueous NaHCO3 and EtOAc were added. The aqueous layer was extracted with EtOAc, and the combined organic layers were dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel chromatography (0-100% EtOAc in hexanes) to give the title compound.

1. temperatureThe mixture was cooled to 0° C.
2. extractionThe aqueous layer was extracted with EtOAc
3. dry with materialthe combined organic layers were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by silica gel chromatography (0-100% EtOAc in hexanes)