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

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%).

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

ORDレコード

ord-6443b95ed90b4833a2ab64a8d940ff33

出典データセット

uspto-grants-2009_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07560558B2