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Ethylene Glycol → HCID 21834550, 화합물

HRID 617743
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HRID 617743 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1([C:15]([OH:17])=[O:16])[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][CH2:9]1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:30](O)[CH2:31][OH:32]>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1([C:15]([OH:17])=[O:16])[CH2:9][CH2:10][C:11]2([O:32][CH2:31][CH2:30][O:14]2)[CH2:12][CH2:13]1
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참가 물질

5

반응물 3

HCID 174Ethylene GlycolHCID 521998p-Toluenesulfonic acid monohydrateHCID 219552001-(2-Fluorophenyl)-4-oxocyclohexanecarboxylic acid

생성물 1

HCID 21834550HCID 21834550, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

1-(2-Fluorophenyl)-4-oxocyclohexane-1-carboxylic acid (D20, 16.36 g, 69 mmol) was stirred with toluene-4-sulphonic acid hydrate (0.50 g, 3 mmol) and 1,2-ethanediol (35 ml) at reflux in toluene (500 ml), removing the immiscible 1,2-ethanediol/water distillate via a Dean-Stark trap until the distillate was homogenous. The solution was then evaporated, dissolved in ethyl acetate, washed with water and brine, dried (Na2SO4) and evaporated to give the title compound (19.94 g, quantitative) as an amber syrup, contaminated with some unidentified materials (NMR).

후처리

  1. customremoving the immiscible 1,2-ethanediol/water distillate via a Dean-Stark trap until the distillate
  2. customThe solution was then evaporated
  3. dissolutiondissolved in ethyl acetate
  4. washwashed with water and brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated

출처 및 근거

ORD 기록
ord-4cc8fc5f12bd4585ba65901de5bec013
출처 데이터셋
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05952325

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