反应详情

To a solution of imidazole (400 mg, 5.88 mmol) and K2CO3 (1.22 g, 8.81 mmol) in DMF (19 ml) was added 4-iodobenzyl bromide (1.83 g, 6.17 mol) at RT under protection from light. After stirring for 11.5 h, the reaction mixture was poured into water. The aqueous layer was extracted twice with EtOAc, the combined organic layers were washed with water and brine, dried over Na2SO4, filtered and concentrated. The residue was purified by column chromatography to afford the title compound (757 mg, 2.66 mmol, 45%) as a beige solid. HPLC: EtRet=3.838 min; LC-MS: m/z 285.2 [M+H]+.

1. extractionThe aqueous layer was extracted twice with EtOAc
2. washthe combined organic layers were washed with water and brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by column chromatography