HRID1984286

反应详情

EQUATION

反应方程式

HRID 1984286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas heated
  2. temperatureunder reflux for 15 h
  3. temperatureAfter cooling
  4. customthe inorganic material separated by filtration
  5. dissolutionThe filtrate was dissolved in chloroform
  6. washwashed with water
  7. dry with materialbrine and dried (MgSO4)
  8. filtrationfiltered
  9. customthe solvent was evaporated
  10. customto give a brown oily residue
  11. customThe residue was purified by flash chromatography