反应详情

To a solution of 4,5-di-(2,4-dichlorophenyl)imidazole (230 mg, 0.65 mmol) from Step B and methyl iodide (0.062 mL, 1.0 mmol) in DMF (5 mL) was added sodium hydride (60% in mineral oil, 52 mg, 1.3 mmol). The reaction was stirred at rt for 3 hr and was then quenched with aq. sodium bicarbonate and extracted twice with ethyl acetate. The organic layers were washed with brine, dried over sodium sulfate, and evaporated. The residue was purified by flash chromatography (50% ethyl acetate in hexanes) to afford the title compound. HPLC/MS: 371 (M+1), 373 (100%, M+3), 375 (M+5); Rt=2.85 min.

1. customwas then quenched with aq. sodium bicarbonate
2. extractionextracted twice with ethyl acetate
3. washThe organic layers were washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated
6. customThe residue was purified by flash chromatography (50% ethyl acetate in hexanes)