HRID972953

反应详情

EQUATION

反应方程式

HRID 972953 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3-hydroxy-2-butanone (90g.) ethyl acetoacetate (175g.), absolute ethanol (150 ml.) and anhydrous zinc chloride (100g.) was heated under reflux for 24 hours. The cooled solution was poured into water and extracted with benzene. The benzene extract was washed successively with 30% aqueous sodium bisulfite, 5% sodium hydroxide, dilute hydrochloric acid and finally with water. The solvent was removed and the residual ester saponified with aqueous-alcoholic alkali as in example 18 to yield 149 g. or 96% yield of the 2,4,5-trimethyl-3-furoic acid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 24 hours
  3. extractionextracted with benzene
  4. extractionThe benzene extract
  5. washwas washed successively with 30% aqueous sodium bisulfite, 5% sodium hydroxide, dilute hydrochloric acid and finally with water
  6. customThe solvent was removed
  7. customto yield 149 g