Diethyl Ether → N'-(1-acetylpiperidin-4-ylidene)benzohydrazide

HRID 44646

反応式

HRID 44646 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][C:7](=O)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[C:11]([NH:19][NH2:20])(=[O:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(OCC)C>C(O)C>[C:1]([N:4]1[CH2:9][CH2:8][C:7](=[N:20][NH:19][C:11](=[O:18])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 11955BenzoylhydrazineHCID 122563N-Acetyl-4-piperidone

生成物 1

HCID 57531701N'-(1-acetylpiperidin-4-ylidene)benzohydrazide収率 83%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

20 g (0.142 mol) of 1-acetyl-4-piperidone were dissolved in 400 mL of absolute ethanol and 21.2 g (0.156 mol) of benzoylhydrazine were added. The resulting solution was refluxed for 6 hours under stirring. The solvent was then removed in vacuo and the residue partitioned between dichloromethane and water. The organic layer was dried over sodium sulfate and evaporated to dryness. The residue was triturated with diethylether and 30 g (83% yield) of the title compound were collected by filtration.

後処理

  1. temperatureThe resulting solution was refluxed for 6 hours
  2. customThe solvent was then removed in vacuo
  3. customthe residue partitioned between dichloromethane and water
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-d168168c723d46c08635a1699a165a5d
出典データセット
uspto-grants-2013_09
特許番号
US08541429B2

関連ノート

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