反応 #75607

ord-4c56a4d91fdb440dbaeedf9e26ebe9cc

反応方程式

[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
収率 49.7%

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was returned to room temperature
  2. 2
    抽出it was extracted with ethyl acetate
  3. 3
    洗浄The organic layer was washed with brine
  4. 4
    乾燥dried over anhydrous sodium sulfate
  5. 5
    その他evaporated
  6. 6
    洗浄The resulting crystalline residue was washed with hexane/ethyl acetate
  7. 7
    ろ過collected by filtration

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06699870B2uspto-grants-2004_03