Methanol → Methyl 4-chloro-2-hydroxybenzoate

HRID 241577

반응식

HRID 241577 반응식
S(=O)(=O)(O)O.[Cl:6][C:7]1[CH:8]=[C:9]([OH:16])[C:10](=[CH:14][CH:15]=1)[C:11]([OH:13])=[O:12].[CH3:17]O>>[Cl:6][C:7]1[CH:8]=[C:9]([OH:16])[C:10](=[CH:14][CH:15]=1)[C:11]([O:13][CH3:17])=[O:12]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 787824-Chlorosalicylic acid

생성물 1

HCID 327085Methyl 4-chloro-2-hydroxybenzoate수율 83%

실험 절차

5 ml of concentrated sulfuric acid is drop-added slowly to 100 ml of methanol. The solution is cooled and then added with a powder of 4-chloro-salicylic acid (17.20 g, 0.1 mol), and a reaction is carried out at reflux for 24 hours. After cooling the reaction, a large amount of deposit precipitates and is filtered out, washed with small amount of methanol, and recrystallized in anhydrous ethanol, to obtain 15.60 g of methyl 4-chloro-salicylate, with a yield of 83%.

후처리

  1. temperatureThe solution is cooled
  2. temperatureat reflux for 24 hours
  3. temperatureAfter cooling
  4. customthe reaction
  5. customa large amount of deposit precipitates
  6. filtrationis filtered out
  7. washwashed with small amount of methanol
  8. customrecrystallized in anhydrous ethanol

출처 및 근거

ORD 기록
ord-466b9f6184ea471992f1f153ca5427a2
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653069B2

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