反应 #4416

ord-81005d9a5e474ae9811ee087317133f2

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed overnight
  2. 2
    其他Solvent was evaporated from the product
  3. 3
    其他the residue was chromatographed twice on silica with the eluant
  4. 4
    其他The first chromatography removed the bulk of the excess piperazine

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.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04725597uspto-grants-1988_02