HRID322995
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 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
- temperatureis refluxed for 30 minutes
- temperaturethen refluxing
- temperaturerefluxing
- concentrationThe reaction is concentrated in vacuo
- customthe residue partitioned between ethyl acetate (100 mL) and water (100 mL)
- washThe organic phase is washed with water (100 mL)
- dry with materialdried o ver magnesium sulphate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give a light brown oil
- washFlash chromatography of the residue eluting with dichloromethane