HRID279570
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux for 2 hours
- customThe volatiles were removed by evaporation
- dissolutionthe residue was dissolved in methylene chloride
- washThe solution was washed with a saturated aqueous sodium hydrogen carbonate solution and brine
- dry with materialdried (MgSO4)
- customthe solvent removed by evaporation
- customThe residue was purified by column chromatography
- washeluting with ethyl acetate/petroleum ether (1/9)