HRID27367

反应详情

EQUATION

反应方程式

HRID 27367 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 2,2'-(4-methoxybenzal)-bis-acetoacetate (30 g), ethanol (450 ml) and 50% sodium hydroxide (450 g) is refluxed vigorously for 1.0 hour. Water (150 ml) is added and most of the ethanol is removed by distillation in vacuo. The concentrate is acidified with concentrated hydrochloric acid and is extracted with ethyl acetate. The ethyl acetate solution is washed with brine, dried, evaporated and the residue is crystallized from benzene-methanol to afford 3.3 g of 3-(4-methoxyphenyl)glutaric acid, melting point 147°-150° C.

WORKUP

后处理

  1. temperatureis refluxed vigorously for 1.0 hour
  2. customis removed by distillation in vacuo
  3. extractionis extracted with ethyl acetate
  4. washThe ethyl acetate solution is washed with brine
  5. customdried
  6. customevaporated
  7. customthe residue is crystallized from benzene-methanol