HRID322995

反应详情

EQUATION

反应方程式

HRID 322995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,4-dibenzyloxyphenol (3.1 g) and sodium hydride (0.44 g, 60% dispersion in mineral oil) in THF (75 mL) is refluxed for 30 minutes then refluxing is allowed to abate. Neat ethyl bromoacetate (1.8 g) is added and refluxing continued for 1 hour. The reaction is concentrated in vacuo and the residue partitioned between ethyl acetate (100 mL) and water (100 mL). The organic phase is washed with water (100 mL), dried o ver magnesium sulphate, filtered and concentrated in vacuo to give a light brown oil. Flash chromatography of the residue eluting with dichloromethane affords ethyl 2,4-dibenzyloxyphenoxyacetate (3.2 g) after trituration with pentane.

WORKUP

后处理

  1. temperatureis refluxed for 30 minutes
  2. temperaturethen refluxing
  3. temperaturerefluxing
  4. concentrationThe reaction is concentrated in vacuo
  5. customthe residue partitioned between ethyl acetate (100 mL) and water (100 mL)
  6. washThe organic phase is washed with water (100 mL)
  7. dry with materialdried o ver magnesium sulphate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customto give a light brown oil
  11. washFlash chromatography of the residue eluting with dichloromethane