HRID457978

反应详情

EQUATION

反应方程式

HRID 457978 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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 Na2SO41 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, 1 H), 7.55–7.52 (m, 2 H), 7.48–7.38 (m, 3 H), 6.89 (d, J=11.7 Hz, 1H), 4.12 (s, 3H).

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated
  2. addition2N HCl was added
  3. additionThe aqueous layer was diluted with ether
  4. customThe organic layer was separated
  5. customdried over Na2SO41
  6. filtrationfiltered
  7. concentrationconcentrated