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2-Acetoxybenzoyl chloride → 4-Diethylaminoethyl-3-phenyl-1-(o-acetoxy benzoyl)piperazine

HRID 596865
ノート
印刷プレビュー

反応式

HRID 596865 の反応式
C(N(CC)[CH:4]([N:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH:7]1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[CH3:5])C.[C:20]([O:23][C:24]1[C:25](=[CH:29][CH:30]=[CH:31][CH:32]=1)[C:26](Cl)=[O:27])(=[O:22])[CH3:21]>C(C(C)=O)C>[CH2:4]([N:6]([CH2:5][CH2:4][N:6]1[CH2:11][CH2:10][N:9]([C:26](=[O:27])[C:25]2[CH:29]=[CH:30][CH:31]=[CH:32][C:24]=2[O:23][C:20](=[O:22])[CH3:21])[CH2:8][CH:7]1[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)[CH2:7][CH3:8])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 796682-Acetoxybenzoyl chlorideHCID 21448529HCID 21448529、化合物

生成物 1

HCID 214485624-Diethylaminoethyl-3-phenyl-1-(o-acetoxy benzoyl)piperazine

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒2 回

実験手順

4-Diethylaminoethyl-3-phenyl-1-(o-acetoxy benzoyl)piperazine is prepared by boiling under reflux 15 g. of 1-diethylaminoethyl-2-phenyl-piperazine dissolved in 100 ml. of methyl ethyl ketone with 11 g. of acetyl salicyclic acid chloride dissolved in 50 ml. methyl ethyl ketone, for 6 hours. The solvent is removed by distillation. The residue is dissolved in water. The aqueous solution is extracted with benzene. Ammonia is added to the aqueous layer until its reaction is alkaline and the thus precipitated oil is extracted with benzene. The benzene extract is dried by means of potassium carbonate and the benzene is distilled off. The residue is distilled in a vacuum. Boiling point: 190° C./0.01 mm. (bath temperature). Light yellow, viscous oil.

後処理

  1. temperatureunder reflux 15 g
  2. customThe solvent is removed by distillation
  3. dissolutionThe residue is dissolved in water
  4. extractionThe aqueous solution is extracted with benzene
  5. additionAmmonia is added to the aqueous layer until its reaction
  6. extractionthe thus precipitated oil is extracted with benzene
  7. extractionThe benzene extract
  8. dry with materialis dried by means of potassium carbonate
  9. distillationthe benzene is distilled off
  10. distillationThe residue is distilled in a vacuum

出典と根拠

ORDレコード
ord-1feae2261fac414b961273cab385a78c
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04012389

反応ノート

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