反应详情

温度

80 °C

3-Chloro-4-fluoro-phenylboronic acid (3.2 g, 18.4 mmol), 5-bromo-2-hydroxy-benzoic acid (4.0 g, 18.4 mmol), and Pd (PPh3)4 (1.67 g, 1.84 mmol) were dissolved in 250 mL of DME, a 1 M Na2CO3 solution (46 mL, 46.0 mmol) added and the mixture heated to 80° C. for 20 h. The reaction mixture was filtered, partially evaporated and EtOAc (200 mL) and 1 N HCl (100 mL) added. The organic layer washed with 1N HCl and saturated sodium bicarbonate, dried over sodium sulfate, and evaporated. The crude material was filtered through a silica plug (THF) to give 3′-chloro-4′-fluoro-4-hydroxy-biphenyl-3-carboxylic acid (2.15 g).

1. filtrationThe reaction mixture was filtered
2. custompartially evaporated
3. additionEtOAc (200 mL) and 1 N HCl (100 mL) added
4. washThe organic layer washed with 1N HCl and saturated sodium bicarbonate
5. dry with materialdried over sodium sulfate
6. customevaporated
7. filtrationThe crude material was filtered through a silica plug (THF)