반응 #4416

ord-81005d9a5e474ae9811ee087317133f2

반응 방정식

ClCCCCc1ccc(Cl)cc1
4-(4-chlorophenyl)butyl chloride
C1CNCCN1
piperazine
Clc1ccc(CCCCN2CCNCC2)cc1
1-[4-(4-chlorophenyl)butyl]piperazine
수율 46.3%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed overnight
  2. 2
    기타Solvent was evaporated from the product
  3. 3
    기타the residue was chromatographed twice on silica with the eluant
  4. 4
    기타The first chromatography removed the bulk of the excess piperazine

실험 절차

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.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04725597uspto-grants-1988_02