HRID985526

反应详情

EQUATION

反应方程式

HRID 985526 的结构方程式

PROCEDURE

实验过程

4-Chloropyridine-2-carboxylic acid methyl ester hydrochloride (25 g, 0.12 mol) was dissolved in methanol (200 ml) and heated at reflux for 66 h. The solvent was evaporated and the residue partitioned between dichloromethane and saturated sodium hydrogencarbonate solution. The organic layer was washed with brine, dried over sodium sulphate and concentrated to give 4-methoxypyridine-2-carboxylic acid methyl ester (17.6 g, 88%) as a yellow crystalline solid. 1H NMR (360 MHz, CDCl3) δH 3.91 (3H, s), 4.02 (3H, s), 6.98 (1H, dd, J 3 and 6), 7.67 (1H, d, J 3), 8.54 (1H, d, J 6).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 66 h
  3. customThe solvent was evaporated
  4. customthe residue partitioned between dichloromethane and saturated sodium hydrogencarbonate solution
  5. washThe organic layer was washed with brine
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated