HRID2116765

反应详情

EQUATION

反应方程式

HRID 2116765 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To ethyl 4-(2-pyrrolidon-1-yl)cyclohexylcarboxylate (5.0 g, mixture of cis and trans isomers, cis:trans=61:39) are added ethanol (25.0 mL, 5V/W) and sodium ethoxide (2.0 equiv. 0.0132 mol), and the mixture is stirred at room temperature for 20 hours. After adding water (5.0 mL, 1V/W), the reaction solution is stirred at room temperature for 2 hours, and evaporated to remove ethanol under reduced pressure. The residue is acidified by adding 2 N hydrochloric acid, and thereto is added an excessive amount of crystalline sodium chloride followed by extraction with methylene chloride. The extract is dried, and evaporated to remove the solvent under reduced pressure. The resulting crystals are collected with toluene to give 4-(2-pyrrolidon-1-yl)cyclohexylcarboxylic acid (2.9 g, trans:cis=88:12, yield 58%).

WORKUP

后处理

  1. stirringthe reaction solution is stirred at room temperature for 2 hours
  2. customevaporated
  3. customto remove ethanol under reduced pressure
  4. additionby adding 2 N hydrochloric acid
  5. additionis added an excessive amount of crystalline sodium chloride
  6. extractionfollowed by extraction with methylene chloride
  7. customThe extract is dried
  8. customevaporated
  9. customto remove the solvent under reduced pressure
  10. customThe resulting crystals are collected with toluene