Iodine → 2-Iodo-4,5-dimethylphenol

HRID 228686

반응식

HRID 228686 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[CH:6][C:7]=1[CH3:8].[I:10]I.S([O-])([O-])=O.[Na+].[Na+]>CO.O>[I:10][C:5]1[CH:6]=[C:7]([CH3:8])[C:2]([CH3:1])=[CH:3][C:4]=1[OH:9]

참가 물질

5

반응물 3

HCID 807IodineHCID 72493,4-DimethylphenolHCID 24437Sodium Sulfite

생성물 1

HCID 136352572-Iodo-4,5-dimethylphenol수율 64%

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

3,4-Dimethylphenol (0.68 g) and iodine (1.82 g) were dissolved in methanol/water (10 ml/5 ml), and the mixture was stirred at room temperature overnight. An aqueous sodium sulfite solution was added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by column chromatography using ethyl acetate-hexane to give 2-iodo-4,5-dimethylphenol (833 mg, yield 64%).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was then washed with water
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. customThe solvent was removed by distillation under the reduced pressure
  5. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-3986cdf6743c42169ba8bf3e20a19168
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560558B2

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