4-Piperidinecarboxamide → 1-Benzylpiperidine-4-carboxamide

HRID 47329

反応式

HRID 47329 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 7831561-Benzylpiperidine-4-carboxamide収率 49.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

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.

後処理

  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

出典と根拠

ORDレコード
ord-4c56a4d91fdb440dbaeedf9e26ebe9cc
出典データセット
uspto-grants-2004_03
特許番号
US06699870B2

関連ノート

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