4-Piperidinecarboxamide → 1-Benzylpiperidine-4-carboxamide

HRID 239105

反応式

HRID 239105 の反応式
[CH2:1](Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH:9]1[CH2:14][CH2:13][CH:12]([C:15]([NH2:17])=[O:16])[CH2:11][CH2:10]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:1]([N:9]1[CH2:14][CH2:13][CH:12]([C:15]([NH2:17])=[O:16])[CH2:11][CH2:10]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 37724-PiperidinecarboxamideHCID 7503Benzyl ChlorideHCID 11430Potassium Carbonate

生成物 1

HCID 7831561-Benzylpiperidine-4-carboxamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

10.2 mL benzylchloride was added to 10 g piperidine-4-carboxylic acid amide and 21.6 g potassiumcarbonate in 280 mL DMF at 5° C. The reaction was stirred over night at RT. The solvent was removed and the residue was dissolved in water and dichlormethane. The organic layer was separated and evaporated. The residue was purified by column chromatographie (silica gel, eluent: dichlormethane/methanol 95:5 to 90:10) to give 9.8 g of the desired product.

後処理

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in water
  3. customThe organic layer was separated
  4. customevaporated
  5. customThe residue was purified by column chromatographie (silica gel, eluent: dichlormethane/methanol 95:5 to 90:10)

出典と根拠

ORDレコード
ord-d51ef4104a7f48138255f28aebcc2c3c
出典データセット
uspto-grants-2014_02
特許番号
US08642774B2

関連ノート

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