Reaktion #56402

ord-699b85be31244c90849a82aab9a3aa96

Reaktionsgleichung

Cc1ccc(S(=O)(=O)O)cc1
4-methylbenzenesulfonic acid
O=C1CCN(Cc2ccccc2)CC1
1-(phenylmethyl)-4-piperidinone
Nc1cccnc1
3-pyridinamine
Cc1ccccc1
methylbenzene
c1ccc(CN2CCC(=Nc3cccnc3)CC2)cc1
N-[1-(phenylmethyl)-4-piperidinylidene]-3-pyridinamine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxed for 5 hours
  2. 2
    Sonstige(The reaction vessel is provided
  3. 3
    Temperaturwith reflux-condensor
  4. 4
    SonstigeAfter the calculated amount of water is separated
  5. 5
    Sonstigethe solvent is evaporated
  6. 6
    workup.DISSOLUTIONThe oily residue is dissolved in 800 parts of 2,2'-oxybispropane
  7. 7
    Sonstigeevaporated again

Vorschrift

A mixture of 19 parts of 1-(phenylmethyl)-4-piperidinone, 11.8 parts of 3-pyridinamine, 120 parts of methylbenzene and a small volume of 4-methylbenzenesulfonic acid is stirred and refluxed for 5 hours. (The reaction vessel is provided with reflux-condensor and water-separator). After the calculated amount of water is separated, the solvent is evaporated. The oily residue is dissolved in 800 parts of 2,2'-oxybispropane and evaporated again, yielding 27 parts of N-[1-(phenylmethyl)-4-piperidinylidene]-3-pyridinamine as a yellow-brown oil.

Quelle

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