HRID236837

反应详情

EQUATION

反应方程式

HRID 236837 的结构方程式

PROCEDURE

实验过程

Powdered ethyl α,β-dibromo-β-(3-chloro-4-cyclohexyl)propionate (33.0 g.) is added portion-wise to 20% ethanolic potassium hydroxide (135 ml) at room temperature. The mixture is refluxed on a steam bath for 6 hours. The alcohol is evaporated and the residue is dissolved in water and covered with ether and is acidified with cold, dilute hydrochloric acid. The ether layer is washed with water, saline, and dried over sodium sulfate. The ether is removed to give a residue which is triturated with carbon tetrachloride. Recrystallization is carried out from acetic acid-water. This material is digested and triturated with boiling carbon tetrachloride to give 3-chloro-4-cyclohexylpropiolic acid.

WORKUP

后处理

  1. temperatureThe mixture is refluxed on a steam bath for 6 hours
  2. customThe alcohol is evaporated
  3. dissolutionthe residue is dissolved in water
  4. washThe ether layer is washed with water, saline
  5. dry with materialdried over sodium sulfate
  6. customThe ether is removed
  7. customto give a residue which
  8. customis triturated with carbon tetrachloride
  9. customRecrystallization
  10. customtriturated with boiling carbon tetrachloride