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2,2,2-Trifluoro-1-(2-fluoro-4-iodopyridin-3-yl)ethanol → 2,2,2-Trifluoro-1-(2-fluoro-4-iodopyridin-3-yl)ethanone

HRID 1920879
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HRID 1920879 반응식
[F:1][C:2]([F:14])([F:13])[CH:3]([C:5]1[C:6]([F:12])=[N:7][CH:8]=[CH:9][C:10]=1[I:11])[OH:4]>C1(C)C=CC=CC=1.[O-2].[Mn+4].[O-2]>[F:14][C:2]([F:1])([F:13])[C:3]([C:5]1[C:6]([F:12])=[N:7][CH:8]=[CH:9][C:10]=1[I:11])=[O:4]
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참가 물질

4

반응물 1

HCID 579697722,2,2-Trifluoro-1-(2-fluoro-4-iodopyridin-3-yl)ethanol

생성물 1

HCID 579695632,2,2-Trifluoro-1-(2-fluoro-4-iodopyridin-3-yl)ethanone수율 89.4%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 1140Toluene용매

실험 절차

2,2,2-trifluoro-1-(2-fluoro-4-iodo-3-pyridyl)ethanol (45 g, 140.2 mmol) was dissolved in anhydrous toluene (1 L). Manganese (IV) oxide (143.4 g, 1.402 mol) was added portionwise with rapid stirring. The mixture was heated to reflux for 3 hours and then allowed to cool and filtered through a plug of celite. The solid residues were washed with EtOAc and the filtrate was concentrated to a deep red oil which was slurried in petrol and then filtered to give a white solid impurity. The filtrate was concentrated to give the product as a red oil (40 g, 89% Yield).

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 3 hours
  3. temperatureto cool
  4. filtrationfiltered through a plug of celite
  5. washThe solid residues were washed with EtOAc
  6. concentrationthe filtrate was concentrated to a deep red oil which
  7. filtrationfiltered
  8. customto give a white solid impurity
  9. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-952b612b903e466dbd0061f47c3a945f
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08173635B2

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