反应详情

To a solution of 2-(4-phenyl-1H-imidazol-1-yl)ethanol (500 mg, 2.66 mmol, 1 eq) in DCM (10 mL) was added PPh3 (778 mg, 2.96 mmol, 1.1 eq), imidazole (203 mg, 2.98 mmol, 1.1 eq) and iodine (753 mg, 2.97 mmol, 1.1 eq). The reaction mixture was allowed to stir at RT overnight. The organic layer was extracted with 1N HCl. The combined acid extracts were then adjusted to pH˜8 with solid sodium carbonate. The aqueous layer was extracted 2× with Et2O. The combined ether extracts were dried over sodium sulfate, filtered and concentrated to dryness to give 1-(2-iodoethyl)-4-phenyl-1H-imidazole (623 mg, 78% yield) which was used without further purification. LC-MS M+H+298.9.

1. extractionThe organic layer was extracted with 1N HCl
2. extractionThe aqueous layer was extracted 2× with Et2O
3. dry with materialThe combined ether extracts were dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated to dryness