Reaktion #75607

ord-4c56a4d91fdb440dbaeedf9e26ebe9cc

Reaktionsgleichung

[Na+].[OH-]
sodium hydroxide
NC(=O)C1CCNCC1
4-piperidinecarboxamide
ClCc1ccccc1
benzyl chloride
O=C([O-])[O-].[K+].[K+]
potassium carbonate
NC(=O)C1CCN(Cc2ccccc2)CC1
1-benzyl-4-piperidine carboxamide
Ausbeute 49.7%

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewas returned to room temperature
  2. 2
    Extraktionit was extracted with ethyl acetate
  3. 3
    WaschenThe organic layer was washed with brine
  4. 4
    Trocknendried over anhydrous sodium sulfate
  5. 5
    Sonstigeevaporated
  6. 6
    WaschenThe resulting crystalline residue was washed with hexane/ethyl acetate
  7. 7
    Filtrationcollected by filtration

Vorschrift

A mixture of 15 g 4-piperidinecarboxamide, 16.3 g benzyl chloride, 32.3 g potassium carbonate and 200 ml N,N-dimethylformamide was stirred at 80° C. for 4 hr. The reaction solution was returned to room temperature, and aqueous sodium hydroxide was added thereto, and then it was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and then evaporated. The resulting crystalline residue was washed with hexane/ethyl acetate and collected by filtration. 12.7 g of 1-benzyl-4-piperidine carboxamide was obtained as white flaky crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06699870B2uspto-grants-2004_03