反应详情

温度

120 °C

To a solution of methyl-3-bromo-4-fluoro benzoate (20 g, 86 mmol) and 4-chlorophenol (11.0 g, 171 mmol) in dimethylsulfoxide (500 mL) was added potassium tert-butoxide (19.3 g, 171 mmol) and the reaction mixture was stirred at 120° C. for 16 hours and then poured into 500 mL of water and extracted with dichloromethane (3×100 mL). The combined extracts were dried over anhydrous sodium sulfate, filtered and evaporated in vacuo. The residue was purified via column chromatography on silica gel (1:1 petroleum ether:EtOAc) to yield 18 g (55 mmol) of 3-bromo-4-(4-chlorophenoxy)-benzoic acid and 2 g of the title compound.

1. extractionextracted with dichloromethane (3×100 mL)
2. dry with materialThe combined extracts were dried over anhydrous sodium sulfate
3. filtrationfiltered
4. customevaporated in vacuo
5. customThe residue was purified via column chromatography on silica gel (1:1 petroleum ether:EtOAc)