HRID1593608

反应详情

EQUATION

反应方程式

HRID 1593608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Cyclohexanonecarboxylic acid ethyl ester (77 g, 450 mmol) and 4-fluorophenylhydrazine hydrochloride (72 g, 443 mmol) were refluxed in 1.25 L of anhydrous ethanol overnight. The resulting yellow solution was cooled, crystals filtered, the filtrate evaporated, the residue partitioned between ethyl acetate and water, organic layer dried over sodium sulfate, evaporated, crystallized from ethyl acetate/heptane to give 113 g (98%) of the desired product.

WORKUP

后处理

  1. temperatureThe resulting yellow solution was cooled
  2. filtrationcrystals filtered
  3. customthe filtrate evaporated
  4. customthe residue partitioned between ethyl acetate and water, organic layer
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customcrystallized from ethyl acetate/heptane