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Sulfuric Acid → 6-Methoxy-benzofuran-2,3-dicarboxylic acid diethyl ester

HRID 1804786
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인쇄 미리보기

반응식

HRID 1804786 반응식
[CH2:1]([O:3][C:4](=[O:22])[CH:5]([O:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH3:21])[CH:15]=1)[C:6](=O)[C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH3:2].S(=O)(=O)(O)O>>[CH2:1]([O:3][C:4]([C:5]1[O:13][C:14]2[CH:15]=[C:16]([O:20][CH3:21])[CH:17]=[CH:18][C:19]=2[C:6]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:22])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 1118Sulfuric AcidHCID 591526762-(3-Methoxy-phenoxy)-3-oxo-succinic acid diethyl ester

생성물 1

HCID 591526576-Methoxy-benzofuran-2,3-dicarboxylic acid diethyl ester

실험 절차

2-(3-Methoxy-phenoxy)-3-oxo-succinic acid diethyl ester (23) (60 g, 193.4 mmol) is dissolved in 32 ml of cooled (−15° C.) cone, sulfuric acid and stirred for 3 h whereas the reaction mixture slowly warmed up to room temperature. Then the mixture is poured onto 1 kg of ice and extracted with diethyl ether. The organic layers are washed with brine, dried over sodium sulfate, filtrated and evaporated. The crude product is purified by Flash-chromatography (silica gel, ethyl acetate/hexanes 1:9).

후처리

  1. extractionextracted with diethyl ether
  2. washThe organic layers are washed with brine
  3. dry with materialdried over sodium sulfate
  • filtrationfiltrated
  • customevaporated
  • customThe crude product is purified by Flash-chromatography (silica gel, ethyl acetate/hexanes 1:9)
  • 출처 및 근거

    ORD 기록
    ord-f01c316d4f3a497b9737865941191e58
    출처 데이터셋
    uspto-grants-2013_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08354431B2

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