反应详情

To a stirring solution of 6-fluoro-4-methoxy-biphenyl-3-carboxylic acid methyl ester (0.5 g, 2.3 mmol) in dioxane (8 mL, 0.3 M) was added 2N NaOH (6.0 mL, 12 mmol). After one'hour at room temperature, the reaction mixture was concentrated, and 2N HCl was added. The aqueous layer was diluted with ether. The organic layer was separated, dried over Na2SO4, filtered and concentrated to afford a 6-fluoro-4-methoxy-biphenyl-3-carboxylic acid (0.55 g, 96%) as a pale yellow powder: Rf 0.18 (5% methanol in dichloromethane); 1H NMR (CDCl3, 300 MHz) δ 8.35 (d, J=9.0 Hz, 1H), 7.55-7.52 (m, 2H), 7.48-7.38 (m, 3H), 6.89 (d, J=11.7 Hz, 1H), 4.12 (s, 3H).

1. customAfter one'hour at room temperature
2. concentrationthe reaction mixture was concentrated
3. addition2N HCl was added
4. additionThe aqueous layer was diluted with ether
5. customThe organic layer was separated
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated