Sulfuric Acid → 3-Amino-2,4-dimethylphenol

HRID 579972노트

반응식

HRID 579972 반응식
C([NH:4][C:5]1[C:6]([CH3:13])=[C:7]([OH:12])[CH:8]=[CH:9][C:10]=1[CH3:11])(=O)C.S(=O)(=O)(O)O>C(O)C>[NH2:4][C:5]1[C:6]([CH3:13])=[C:7]([OH:12])[CH:8]=[CH:9][C:10]=1[CH3:11]

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 10419764N-(3-Hydroxy-2,6-dimethylphenyl)acetamide

생성물 1

HCID 141306083-Amino-2,4-dimethylphenol수율 69.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 10 g of 3-acetamido-2,4-dimethylphenol (55.9 mmol), 250 ml of concentrated sulfuric acid and 200 ml of ethanol was refluxed for 30 minutes and, then, concentrated under reduced pressure. The residue was dissolved in water and the solution was made alkaline with ammonia water and extracted with ether. The ether layer was washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate (dehydration) and concentrated under reduced pressure. The residue was recrystallized from ethanolhexane to give 5.3 g (69%) of the title compound as colorless plates, m.p. 177°-179° C.

후처리

  1. temperaturewas refluxed for 30 minutes
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in water
  4. extractionextracted with ether
  5. washThe ether layer was washed with a saturated aqueous solution of sodium chloride
  6. dry with materialdried over magnesium sulfate (dehydration)
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was recrystallized from ethanolhexane

출처 및 근거

ORD 기록
ord-0564bda8e7404383b919e8d4ec3a662c
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04751232

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