反応 #2324

ord-53468aff36b74b69af45a0218b9d4c73

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他to reach ambient temperature
  2. 2
    その他the organic phase separated
  3. 3
    その他dried
  4. 4
    その他(MgSO4), and removal of the solvent
  5. 5
    その他by evaporation

実験手順

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)+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05728701uspto-grants-1998_03