HRID2376001

反应详情

EQUATION

反应方程式

HRID 2376001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 1-chloro-3-(triphenylphosphoranylidene)acetone (6.6 g) and ethyl glyoxylate (50% in toluene, 4.6 g) in dioxane (66 mL) was stirred at 80′ for 1.5 hour. The solvent was removed by concentration. The residue was purified by column chromatography on silica gel using a mixture of chloroform and hexane (1:1 v/v) as an eluent. The eluted fractions containing the desired product were collected and evaporated in vacuo to give ethyl (2E)-5-chloro-4-oxo-2-pentenoate (1.58 g).

WORKUP

后处理

  1. customThe solvent was removed by concentration
  2. customThe residue was purified by column chromatography on silica gel using
  3. additiona mixture of chloroform and hexane (1:1 v/v) as an eluent
  4. additionThe eluted fractions containing the desired product
  5. customwere collected
  6. customevaporated in vacuo