HRID1109481

反应详情

EQUATION

反应方程式

HRID 1109481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

8 g of 1-[4-aminobenzoyl]-4-[2-(4-chlorophenyl)ethyl]-piperazine are dissolved in 200 ml of dioxane. 8.7 g of chloroformic acid benzyl ester in the form of a 50% solution in toluene are added dropwise thereto at 15°. After 2 hours at room temperature, the reaction mixture is diluted with water, dioxane is distilled off and the aqueous phase is rendered alkaline with 2N sodium hydroxide solution and extracted by shaking with ethyl acetate. The oil obtained from the ethyl acetate is crystallised from alcohol and ether, yielding 1-[4-(N-benzyloxycarbonylamino)benzoyl]-4-[2-(4-chlorophenyl)ethyl]-piperazine having a melting point of 149°-150°.

WORKUP

后处理

  1. customat 15°
  2. distillationis distilled off
  3. extractionextracted
  4. customThe oil obtained from the ethyl acetate
  5. customis crystallised from alcohol and ether