Piperazine → Piperazine,1-[4-(4-chlorophenyl)butyl]-

HRID 4320

Reaktionsgleichung

Reaktionsgleichung von HRID 4320
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][CH2:11]Cl)=[CH:4][CH:3]=1.[NH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][CH2:11][N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 4837PiperazineHCID 200827321-Chloro-4-(4-chlorobutyl)benzene

Produkt 1

HCID 14097058Piperazine,1-[4-(4-chlorophenyl)butyl]-Ausbeute 46,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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.).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-81005d9a5e474ae9811ee087317133f2
Quelldatensatz
uspto-grants-1988_02
Patentnummer
US04725597

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