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Methyl iodide → 1-Benzyl 3-ethyl 3-methyl-4-oxopyrrolidine-1,3-dicarboxylate

HRID 480401
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HRID 480401 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH:14]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:13](=[O:21])[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:22](=O)([O-])[O-].[K+].[K+].IC>CC(C)=O>[CH2:1]([O:8][C:9]([N:11]1[CH2:15][C:14]([C:16]([O:18][CH2:19][CH3:20])=[O:17])([CH3:22])[C:13](=[O:21])[CH2:12]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

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 150432781-Benzyl 3-ethyl 4-oxopyrrolidine-1,3-dicarboxylate

생성물 1

HCID 572801371-Benzyl 3-ethyl 3-methyl-4-oxopyrrolidine-1,3-dicarboxylate수율 80.7%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To the solution of N-benzyloxycarbonyl-4-ethoxycarbonylpyrrolidin-3-one (291 g) in acetone (1.5 l) was added potassium carbonate (200 g), followed by iodomethane (300 mL), and then the solution was refluxed for 3 hr. The reaction mixture was cooled at room temperature, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate: n-hexane=1:6) to obtain the desired compound (237.7 g, 80.7%).

후처리

  1. temperaturethe solution was refluxed for 3 hr
  2. filtrationfiltered
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate: n-hexane=1:6)

출처 및 근거

ORD 기록
ord-5af1f80d201e478dbe2d0ea822f052f0
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06649763B1

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