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Potassium Acetate → Ethyl 2-(1-benzyloxycarbonyl-3-azetidinyl)acrylate

HRID 1457998
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HRID 1457998 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:14][CH:13]([CH:15]([C:21](O)=O)[C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])(=O)C.[K+]>C(#N)C>[CH2:1]([O:8][C:9]([N:11]1[CH2:12][CH:13]([C:15](=[CH2:21])[C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:14]1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 517044Potassium AcetateHCID 53765389Ethyl hydrogen (1-benzyloxycarbonyl-3-azetidinyl)malonate

생성물 1

HCID 54322358Ethyl 2-(1-benzyloxycarbonyl-3-azetidinyl)acrylate수율 86.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To 732 mg (2.28 mmol) of ethyl hydrogen (1-benzyloxycarbonyl-3-azetidinyl)malonate dissolved in 70 ml of acetonitrile were added 1.05 g (5.67 mmol) of Eshenmoser's salt and a catalytically effective amount of potassium acetate, followed by 4.5 hours of heating under reflux. After evaporation of the solvent, the resulting residue was mixed with 100 ml of ethyl acetate, washed with 10% citric acid aqueous solution, 10% sodium sulfite aqueous solution and saturated brine in that order, and then dried over anhydrous sodium sulfate. By evaporating the solvent, 569 mg (86%) of the title compound was obtained.

후처리

  1. additionwere added 1.05 g (5.67 mmol) of Eshenmoser's salt
  2. temperatureof heating
  3. temperatureunder reflux
  4. customAfter evaporation of the solvent
  5. additionthe resulting residue was mixed with 100 ml of ethyl acetate
  6. washwashed with 10% citric acid aqueous solution, 10% sodium sulfite aqueous solution and saturated brine in that order
  7. dry with materialdried over anhydrous sodium sulfate
  8. customBy evaporating the solvent

출처 및 근거

ORD 기록
ord-811ea7ee01dd4281abbeeec749354545
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05849757

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