反应详情

To a solution of 4-phenyl-1H-imidazole (1 g, 8.75 mmoles) in DMF (8 mL) is added NaH 60% dispersion in mineral oil (455 mg, 11 mmoles). The reaction mixture is stirred at room temperature for 1 hour, then methanesulfonic acid phenethyl ester (example 4D) (1.84 g, 9.12 mmoles) is added. The reaction mixture is then heated at 60° C. for 2 hours. Water is added, and the aqueous phase is extracted three times with AcOEt. The organic phase is washed with water, brine, dried over magnesium sulphate, filtered and the solvent is removed under reduced pressure. The residue is purified by silica gel chromatography using (CH2Cl2:MeOH) (100:0) then (98:2) to give 1-phenethyl-4-phenyl-imidazole.

1. temperatureThe reaction mixture is then heated at 60° C. for 2 hours
2. extractionthe aqueous phase is extracted three times with AcOEt
3. washThe organic phase is washed with water, brine
4. dry with materialdried over magnesium sulphate
5. filtrationfiltered
6. customthe solvent is removed under reduced pressure
7. customThe residue is purified by silica gel chromatography