HRID2292089

反应详情

EQUATION

反应方程式

HRID 2292089 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A catalytic amount of a 5% strength methanolic sodium methylate solution is added to a mixture of 4.9 g (0.03 mol) of 2-cyano-3-pyridylacetonitrile and 3.4 g (0.03 mol) of methyl crotonate with stirring at a rate such that the reaction temperature remains below 40° C. When the evolution of heat has subsided, the mixture is neutralized using dilute acetic acid. The mixture is extracted with chloroform and the organic phase is dried over MgSO4, filtered and concentrated in vacuo. The residue is purified over a silica gel column using chloroform as eluent.

WORKUP

后处理

  1. customremains below 40° C
  2. temperatureWhen the evolution of heat
  3. extractionThe mixture is extracted with chloroform
  4. dry with materialthe organic phase is dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue is purified over a silica gel column