Reaktion #2324

ord-53468aff36b74b69af45a0218b9d4c73

Reaktionsgleichung

O
Water
CC(=O)Cl
Acetyl chloride
NC1CCN(Cc2ccccc2)CC1
4-amino1-benzylpiperidine
CCN(CC)CC
triethylamine
CC(=O)NC1CCN(Cc2ccccc2)CC1
4-acetylamino-1-benzylpiperidine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto reach ambient temperature
  2. 2
    Sonstigethe organic phase separated
  3. 3
    Sonstigedried
  4. 4
    Sonstige(MgSO4), and removal of the solvent
  5. 5
    Sonstigeby evaporation

Vorschrift

Acetyl chloride (3.95 ml) was added dropwise to a stirred solution of 4-amino1-benzylpiperidine (10.0 g) and triethylamine (7.7 ml) in dry dichloromethane (100 ml) at 4° C. The mixture was allowed to reach ambient temperature and stirred for 16 hours. Water was then added, the organic phase separated and dried (MgSO4), and removal of the solvent by evaporation gave 4-acetylamino-1-benzylpiperidine, 10.23 g, as a light brown solid which was used without further purification: NMR (CDCl3) δ 7.29(5H,m), 5.29(1H,b), 3.79(1H,m), 3.49(2H,s), 2.80(2H,dm), 2.12(2H,dt), 1.95(3H,s), 191(2H,dm), 1.46(2H,dq); m/e 233 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05728701uspto-grants-1998_03