Reaktion #56405

ord-69afb760ce334456b0c8437bc4ff6a35

Reaktionsgleichung

Cc1ccc(S(=O)(=O)O)cc1
4-methylbenzenesulfonic acid
CCOC(=O)N1CCC(=O)CC1
ethyl 4-oxo-1-piperidinecarboxylate
Nc1ccc(Cl)cc1
4-chlorobenzenamine
Cc1ccccc1
methylbenzene
CCOC(=O)N1CCC(=Nc2ccc(Cl)cc2)CC1
ethyl 4-[(4-chlorophenyl)imino]-1-piperidinecarboxylate

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxed for 7 hours
  2. 2
    Sonstige(The reaction vessel is provided with
  3. 3
    Temperatura reflux-condensor
  4. 4
    SonstigeThe methylbenzene is evaporated
  5. 5
    workup.DISTILLATIONthe oily residue is distilled in vacuo

Vorschrift

A mixture of 171.2 parts of ethyl 4-oxo-1-piperidinecarboxylate, 159.5 parts of 4-chlorobenzenamine, 1520 parts of anhydrous methylbenzene and a few crystals of 4-methylbenzenesulfonic acid is stirred and refluxed for 7 hours. (The reaction vessel is provided with a reflux-condensor and water-separator). The methylbenzene is evaporated and the oily residue is distilled in vacuo, yielding 192 parts of oily ethyl 4-[(4-chlorophenyl)imino]-1-piperidinecarboxylate; bp. 171°-176° C. at 0.4 mm. pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04225606uspto-grants-1980_09