反应详情

To a solution of 2-fluoro-3-iodo-5-methoxy-benzoic acid (3.0 g 10.14 mmol, 1.0 eq) in a mixture of water (30 mL), EtOH (30 mL) and DMF (60 mL), was added 3-fluorophenylboronic acid (1.56 g 11.15 mmol, 1.1 eq) and Na2CO3 (4.3 g, 40.56 mmol, 4.0 eq). The mixture was stirred at room temperature under N2 for 10 mins then Pd(PPh3)4 (1.17 g, 1.01 mmol, 0.1 eq) was added. The mixture was heated at 100° C. for 5 h then cooled to room temperature and acidified with 1M HCl. The aqueous layer was extracted with EtOAc and the combined extracts were washed with water, dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:3) to give the title compound as a yellow solid (2.2 g, 81%).

1. temperatureThe mixture was heated at 100° C. for 5 h
2. temperaturethen cooled to room temperature
3. extractionThe aqueous layer was extracted with EtOAc
4. washthe combined extracts were washed with water
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customevaporated in vacuo
8. customThe residue was purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:3)