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Acetic Acid → 2,3-Difluoro-4-hydroxybenzoic acid

HRID 1166716
ノート
印刷プレビュー

反応式

HRID 1166716 の反応式
[F:1][C:2]1[C:7]([F:8])=C(C#N)[CH:5]=[CH:4][C:3]=1[OH:11].[C:12]([OH:15])(=[O:14])[CH3:13]>O.OS(O)(=O)=O>[F:8][C:7]1[C:2]([F:1])=[C:3]([OH:11])[CH:4]=[CH:5][C:13]=1[C:12]([OH:15])=[O:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 176Acetic AcidHCID 27369782,3-Difluoro-4-hydroxybenzonitrile

生成物 1

HCID 27793072,3-Difluoro-4-hydroxybenzoic acid収率 71%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1118Sulfuric Acid溶媒

実験手順

A mixture of 2,3-difluoro-4-cyanophenol (1 g, 6.45 mmol) in water (8 mL), H2SO4 (8 mL), and acetic acid (8 mL) was refluxed for 48 hours. The solvents were removed by rotary evaporation to give a slurry which was poured onto ice. The product precipitated out of solution and filtered. The solid was washed with water and dried to give 2,3-difluoro-4-hydroxybenzoic acid (800 mg, 71%).

後処理

  1. temperaturewas refluxed for 48 hours
  2. customThe solvents were removed by rotary evaporation
  3. customto give a slurry which
  4. additionwas poured onto ice
  5. customThe product precipitated out of solution
  6. filtrationfiltered
  7. washThe solid was washed with water
  8. customdried

出典と根拠

ORDレコード
ord-6073920baf8d42518caede8960c366b4
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06613942B1

反応ノート

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