反应 #75607

ord-4c56a4d91fdb440dbaeedf9e26ebe9cc

反应方程式

[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
收率 49.7%

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他was returned to room temperature
  2. 2
    萃取it was extracted with ethyl acetate
  3. 3
    洗涤The organic layer was washed with brine
  4. 4
    干燥dried over anhydrous sodium sulfate
  5. 5
    其他evaporated
  6. 6
    洗涤The resulting crystalline residue was washed with hexane/ethyl acetate
  7. 7
    过滤collected by filtration

实验过程

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.

来源

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