Iodine → 4-(Imidazol-1-yl)-2-iodophenol

HRID 228695

반응식

HRID 228695 반응식
[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.[I:13]I.S([O-])([O-])(=O)=S.[Na+].[Na+]>O.CO.ClCCl>[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([OH:12])=[C:8]([I:13])[CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1

참가 물질

7

반응물 3

HCID 807IodineHCID 24477Sodium ThiosulfateHCID 823151-(p-Hydroxyphenyl)imidazole

생성물 1

HCID 222744934-(Imidazol-1-yl)-2-iodophenol수율 14%

시약·촉매·용매 3

HCID 887Methanol용매2회HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

4-(Imidazol-1-yl)phenol (500 mg) was dissolved in water (6 ml), methanol (18 ml), and dichloromethane (6 ml) to prepare a solution. Iodine (1.58 g) was added to the solution, and the mixture was stirred at room temperature for 8 days. An aqueous sodium thiosulfate solution and methanol were added to the reaction solution, and the mixture was stirred and was then concentrated. The concentrate was extracted with chloroform, and the chloroform layer was then washed with water and saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give 4-(imidazol-1-yl)-2-iodophenol (123 mg, yield 14%).

후처리

  1. stirringthe mixture was stirred
  2. concentrationwas then concentrated
  3. extractionThe concentrate was extracted with chloroform
  4. washthe chloroform layer was then washed with water and saturated brine
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. customThe solvent was removed
  7. distillationby distillation under the reduced pressure
  8. customthe residue was purified by thin layer chromatography

출처 및 근거

ORD 기록
ord-6443b95ed90b4833a2ab64a8d940ff33
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560558B2

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