HRID2225493

反应详情

EQUATION

反应方程式

HRID 2225493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20 ml of a 2N aqueous sodium hydroxide solution was added to a solution of 2.1 g of methyl 4-acetyl-1-methyl-1-cyclohexanecarboxylate (Example 35) in 20 ml of ethanol. The solution was reacted for 4 hours, while it was refluxed. After reaction, 2N hydrochloric acid was added to the reaction solution, acidifying the solution. The solution was extracted three times with 50 ml of ethyl acetate. The organic layer obtained was washed twice with an aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was removed in vacuo, and the product obtained was recrystallized from ethyl acetate/hexane, yielding 1.4 g of 4-acetyl-1-methyl-1-cyclohexanecarboxylic acid as white crystal, which had the following physiochemical properties:

WORKUP

后处理

  1. customThe solution was reacted for 4 hours, while it
  2. temperaturewas refluxed
  3. additionwas added to the reaction solution
  4. extractionThe solution was extracted three times with 50 ml of ethyl acetate
  5. customThe organic layer obtained
  6. washwas washed twice with an aqueous sodium chloride solution
  7. dry with materialdried over magnesium sulfate
  8. customThe solvent was removed in vacuo
  9. customthe product obtained
  10. customwas recrystallized from ethyl acetate/hexane