Ethanol → Ethyl 2-chloro-4-hydroxybenzoate

HRID 1442478

反応式

HRID 1442478 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]([OH:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH2:17](O)[CH3:18]>O>[CH2:17]([O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][C:9]([OH:11])=[CH:10][C:2]=1[Cl:1])[CH3:18]

参加物

5

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 918212-Chloro-4-hydroxybenzoic acid

生成物 1

HCID 19981058Ethyl 2-chloro-4-hydroxybenzoate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution consisting of 34.5 g (200 mmol) of 2-chloro-4-hydroxy-benzoic acid, 5 mL of concentrated sulfuric acid and 400 mL of ethanol was refluxed for 18 hours. 1.2 L of water were added to the resulting mixture followed by extraction with 1.5 L of methylene chloride. The mixture was then washed with aqueous sodium bicarbonate solution and water and dried with magnesium sulfate followed by distilling off the solvent. The residue was recrystallized from hexane/ethyl acetate to obtain 20.4 g of a light orange solid.

後処理

  1. temperaturewas refluxed for 18 hours
  2. extractionfollowed by extraction with 1.5 L of methylene chloride
  3. washThe mixture was then washed with aqueous sodium bicarbonate solution and water
  4. dry with materialdried with magnesium sulfate
  5. distillationby distilling off the solvent
  6. customThe residue was recrystallized from hexane/ethyl acetate

出典と根拠

ORDレコード
ord-22eabb4dce4d4a8ea018e7cf9cb24236
出典データセット
uspto-grants-2010_02
特許番号
US07658979B2

関連ノート

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