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

HRID 596865
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HRID 596865 반응식
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]
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참가 물질

4

반응물 2

HCID 796682-Acetoxybenzoyl chlorideHCID 21448529HCID 21448529, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1feae2261fac414b961273cab385a78c
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04012389

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