HRID129692

反应详情

EQUATION

反应方程式

HRID 129692 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a refluxing suspension of 15.71 g (140 mmol, 1.4 eq) of potassium t-butoxide in 50 ml of t-butylalcohol is dropped in a mixture of 12.17 (100 mmol) of 3-methoxybenzaldehyde and 15.70 ml (120 mmol, 1.2 eq) of dimethyl succinate dissolved in 20 ml of t-butylalcohol. The mixture is refluxed for 3 hours, concentrated in vacuo, acidified to pH ~1 using 1N HCl, and extracted with ethylacetate. The organics are dried (MgSO4) and concentrated in vacuo to give 3-carbomethoxy-4-(3-methoxyphenyl)-3-butenoic acid in the form of a yellow oil which is used directly in the next step.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 3 hours
  2. concentrationconcentrated in vacuo
  3. extractionextracted with ethylacetate
  4. dry with materialThe organics are dried (MgSO4)
  5. concentrationconcentrated in vacuo