HRID2166706

反应详情

EQUATION

反应方程式

HRID 2166706 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-(2-furanyl)propionate (33.77 g) and ethyl formate (22.22 g) was added dropwise with stirring to a pre-cooled (0° C.) suspension of sodium hydride (50% in oil; 8.45 g) in dimethoxyethane (70 ml) maintaining the temperature below 0° C. throughout the addition. The reaction mixture was allowed to warm to room temperature then poured on to ice and water and extracted with ethyl acetate. The aqueous layer was acidified to pH 4 and re-extracted with ethyl acetate. These second ethyl acetate extracts were combined dried (MgSO4) and evaporated at reduced pressure to yield ethyl 3-(2-furanyl)-2-formylpropionate (19.0 g).

WORKUP

后处理

  1. additionwas added dropwise
  2. temperaturea pre-cooled
  3. temperaturemaintaining the temperature below 0° C.
  4. additionthroughout the addition
  5. extractionextracted with ethyl acetate
  6. extractionre-extracted with ethyl acetate
  7. dry with materialThese second ethyl acetate extracts were combined dried (MgSO4)
  8. customevaporated at reduced pressure