반응 #2324

ord-53468aff36b74b69af45a0218b9d4c73

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타to reach ambient temperature
  2. 2
    기타the organic phase separated
  3. 3
    기타dried
  4. 4
    기타(MgSO4), and removal of the solvent
  5. 5
    기타by evaporation

실험 절차

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)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728701uspto-grants-1998_03