反应详情

To (2′-hydroxymethyl-6-methoxy-4′-trifluoromethyl-biphenyl-3-yl)-acetic acid methyl ester (1.66 g, 4.68 mmol) in DME (17 mL) was added phosphorus tribromide (0.66 mL, 7.03 mmol), and the reaction was stirred at room temperature for 3 hours. The mixture was cooled to 0° C. and quenched with aqueous NaHCO3 and CH2Cl2. The aqueous layer was separated and extracted with CH2Cl2, and the combined organic layers were dried over MgSO4, filtered, and concentrated. The crude material was purified by silica gel chromatography to give the title compound.

1. temperatureThe mixture was cooled to 0° C.
2. customquenched with aqueous NaHCO3 and CH2Cl2
3. customThe aqueous layer was separated
4. extractionextracted with CH2Cl2
5. dry with materialthe combined organic layers were dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude material was purified by silica gel chromatography