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1,2,3-Trimethoxybenzene → 4-Oxo-4-(2,3,4-trimethoxy-phenyl)-butyric acid methyl ester

HRID 1944645
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인쇄 미리보기

반응식

HRID 1944645 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[C:4]=1[O:11][CH3:12].[C:13]([O:20][CH3:21])(=[O:19])[CH2:14][CH2:15][C:16]([O-])=[O:17]>>[CH3:21][O:20][C:13](=[O:19])[CH2:14][CH2:15][C:16](=[O:17])[C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([O:11][CH3:12])[C:5]=1[O:9][CH3:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 124621,2,3-TrimethoxybenzeneHCID 6930703Mono-Methyl Succinate

생성물 1

HCID 447204584-Oxo-4-(2,3,4-trimethoxy-phenyl)-butyric acid methyl ester수율 72.7%

반응 조건

온도
45 °C

실험 절차

A mixture of 75 g of polyphosphoric acid (Acros), 1,2,3-trimethoxybenzene (5.0 g, 29.73 mmol), and mono-methyl succinate (5.9 g, 44.59 mmol) were mechanically stirred at 45° C. for 2.5 h. The reaction mixture was then poured into a 1000 mL beaker containing round 250 mL of ice, and stirred well until all the product was precipitated out. The tan colored product was then filtered and washed with water and dried under vacuum. 6.1 g (72%) of 55 was obtained, which was pure by NMR.

후처리

  • additionThe reaction mixture was then poured into a 1000 mL beaker
  • stirringstirred well until all the product
  • customwas precipitated out
  • filtrationThe tan colored product was then filtered
  • washwashed with water
  • customdried under vacuum
  • 출처 및 근거

    ORD 기록
    ord-0f88c7e6faf14857991989567db2359d
    출처 데이터셋
    uspto-grants-2013_03
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08394859B2

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