Hydrochloric Acid → Methyl 4-chloro-2-hydroxybenzoate

HRID 259668

反応式

HRID 259668 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([OH:12])[C:6](=[CH:10][CH:11]=1)[C:7]([OH:9])=[O:8].[CH3:13]O>>[Cl:2][C:3]1[CH:4]=[C:5]([OH:12])[C:6](=[CH:10][CH:11]=1)[C:7]([O:9][CH3:13])=[O:8]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 787824-Chlorosalicylic acid

生成物 1

HCID 327085Methyl 4-chloro-2-hydroxybenzoate

実験手順

Hydrogen chloride gas is bubbled into a mixture of 4-chlorosalicylic acid (100 g, 0.579 mol) in methanol while maintaining the temperature at 45°-50° C. The reaction mixture is then stirred at room temperature for several hours, concentrated in vacuo and extracted with ether. The combined organic extracts are washed sequentially with brine, saturated sodium hydrogen carbonate solution and brine, dried over anhydrous sodium sulfate and concentrated in vacuo to obtain an amber oil. The oil is distilled under reduced pressure to give the title product as a colorless oil which is identified by NMR spectral analyses.

後処理

  1. temperaturewhile maintaining the temperature at 45°-50° C
  2. concentrationconcentrated in vacuo
  3. extractionextracted with ether
  4. washThe combined organic extracts are washed sequentially with brine, saturated sodium hydrogen carbonate solution and brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customto obtain an amber oil
  8. distillationThe oil is distilled under reduced pressure

出典と根拠

ORDレコード
ord-1e8dce9651a145ceb2753c779256c78f
出典データセット
uspto-grants-1996_06
特許番号
US05523278

関連ノート

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