HRID279570

反应详情

EQUATION

反应方程式

HRID 279570 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-chloro-6-methyl-4-pyridinecarboxylic acid (2 g, 12 mmol) in ethanol (100 ml) and concentrated sulphuric acid (10 ml) was heated at reflux for 2 hours. The volatiles were removed by evaporation and the residue was dissolved in methylene chloride. The solution was washed with a saturated aqueous sodium hydrogen carbonate solution and brine, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by column chromatography eluting with ethyl acetate/petroleum ether (1/9) to give ethyl 2-chloro-6-methyl-4-pyridinecarboxylate (2 g, 86%).

WORKUP

后处理

  1. temperatureat reflux for 2 hours
  2. customThe volatiles were removed by evaporation
  3. dissolutionthe residue was dissolved in methylene chloride
  4. washThe solution was washed with a saturated aqueous sodium hydrogen carbonate solution and brine
  5. dry with materialdried (MgSO4)
  6. customthe solvent removed by evaporation
  7. customThe residue was purified by column chromatography
  8. washeluting with ethyl acetate/petroleum ether (1/9)