HRID45245

反应详情

EQUATION

反应方程式

HRID 45245 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 43.5 g (214 mmol) of ethyl 3-cyano-3-phenylpropanoate and 52.2 g (930.4 mmol) of potassium hydroxide in 670 mL of EtOH is refluxed for 4 hours. After cooling to room temperature, the medium is concentrated under vacuum and then treated with 1 L of 1N HCl, and a precipitate then forms, which is filtered off and rinsed with water (2×50 mL). The solid obtained is taken up in a mixture of 200 mL of toluene and 40 mL of EtOH and concentrated under reduced pressure, and then dried with a vane pump. 37 g of 2-phenylbutanedioic acid are obtained in the form of a solid, which is used without further purification in the following step.

WORKUP

后处理

  1. temperatureis refluxed for 4 hours
  2. concentrationthe medium is concentrated under vacuum
  3. additiontreated with 1 L of 1N HCl
  4. filtrationwhich is filtered off
  5. washrinsed with water (2×50 mL)
  6. customThe solid obtained
  7. concentrationconcentrated under reduced pressure
  8. customdried with a vane pump