4-Piperidinecarboxamide → 1-Benzylpiperidine-4-carboxamide

HRID 47329

반응식

HRID 47329 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([C:7]([NH2:9])=[O:8])[CH2:3][CH2:2]1.[CH2:10](Cl)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+].[OH-].[Na+]>CN(C)C=O>[CH2:10]([N:1]1[CH2:6][CH2:5][CH:4]([C:7]([NH2:9])=[O:8])[CH2:3][CH2:2]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

참가 물질

6

반응물 4

HCID 37724-PiperidinecarboxamideHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 14798Sodium Hydroxide

생성물 1

HCID 7831561-Benzylpiperidine-4-carboxamide수율 49.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

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.

후처리

  1. customwas returned to room temperature
  2. extractionit was extracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated
  6. washThe resulting crystalline residue was washed with hexane/ethyl acetate
  7. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-4c56a4d91fdb440dbaeedf9e26ebe9cc
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699870B2

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