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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 384091
ノート
印刷プレビュー

反応式

HRID 384091 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 1140Toluene溶媒

実験手順

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).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-a22f0e484bec49a4847ffc3c8bddce2b
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367697B2

反応ノート

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