반응 #75607

ord-4c56a4d91fdb440dbaeedf9e26ebe9cc

반응 방정식

[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
수율 49.7%

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was returned to room temperature
  2. 2
    추출it was extracted with ethyl acetate
  3. 3
    세척The organic layer was washed with brine
  4. 4
    건조dried over anhydrous sodium sulfate
  5. 5
    기타evaporated
  6. 6
    세척The resulting crystalline residue was washed with hexane/ethyl acetate
  7. 7
    여과collected by filtration

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06699870B2uspto-grants-2004_03