HRID4320

反应详情

EQUATION

反应方程式

HRID 4320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 26.4 g of 4-(4-chlorophenyl)butyl chloride, 86.1 g of anhydrous piperazine and 250 ml of reagent ethanol was refluxed overnight. Solvent was evaporated from the product and the residue was chromatographed twice on silica with the eluant being CH2Cl2 /CH3OH/ammonium hydroxide (45:5:1). The first chromatography removed the bulk of the excess piperazine, the second provided 15.2 g of 1-[4-(4-chlorophenyl)butyl]piperazine as a colorless oil which solidified on standing (m.p. 139°-145° C.).

WORKUP

后处理

  1. temperaturewas refluxed overnight
  2. customSolvent was evaporated from the product
  3. customthe residue was chromatographed twice on silica with the eluant
  4. customThe first chromatography removed the bulk of the excess piperazine