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Acetic Acid → 5-Methoxy-3-methylbenzofuran

HRID 2091178
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반응식

HRID 2091178 반응식
[C:1]([C:4]1[CH:14]=[C:13]([O:15][CH3:16])[CH:12]=[CH:11][C:5]=1[O:6][CH2:7]C(O)=O)(=O)[CH3:2].C(OC(=O)C)(=O)C.C(O)(=O)C>O>[CH3:16][O:15][C:13]1[CH:12]=[CH:11][C:5]2[O:6][CH:7]=[C:1]([CH3:2])[C:4]=2[CH:14]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 7918Acetic AnhydrideHCID 13156994Acetic acid, 2-(2-acetyl-4-methoxyphenoxy)-

생성물 1

HCID 131569985-Methoxy-3-methylbenzofuran수율 81.1%

시약·촉매·용매 1

HCID 962Water용매

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온도
110 °C

실험 절차

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

A mixture of (2-acetyl-4-methoxyphenoxy)acetic acid (10.0 g) synthesized above, acetic anhydride (18.3 g) and acetic acid (100 mL) was stirred at 110° C. for 5 hr, poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (5% ethyl acetate/hexane) to give the title object compound (5.87 g, 81%) as a colorless oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (5% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-741101901d7541238fe4c451fc6c11a5
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08436043B2

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