HRID1984286
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 mixture of ethyl 3-hydroxy-picolinate (11.0 g, 65.8 mmol), ethyl bromoacetate (12.1 g, 72.4 mmol) and anhydrous potassium carbonate (11.8 g, 85.5 mmol) in acetone (120 mL) was heated under reflux for 15 h. After cooling, the inorganic material separated by filtration. The filtrate was dissolved in chloroform, washed with water, then brine and dried (MgSO4), filtered, and the solvent was evaporated to give a brown oily residue. The residue was purified by flash chromatography using a gradient of ammoniated methanol in chloroform to give ethyl 2-(2-ethoxycarbonyl-3-pyridyloxy)acetate (13.7 g) as a yellow oil (13.7 g).
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 15 h
- temperatureAfter cooling
- customthe inorganic material separated by filtration
- dissolutionThe filtrate was dissolved in chloroform
- washwashed with water
- dry with materialbrine and dried (MgSO4)
- filtrationfiltered
- customthe solvent was evaporated
- customto give a brown oily residue
- customThe residue was purified by flash chromatography