Ethanol → Ethyl 2-chloro-4-hydroxybenzoate

HRID 1442478

반응식

HRID 1442478 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 19981058Ethyl 2-chloro-4-hydroxybenzoate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-22eabb4dce4d4a8ea018e7cf9cb24236
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07658979B2

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