反应详情

温度

80 °C

A mixture of tetrakis(triphenylphosphine)palladium(0) (89 mg), methyl (E)-3-(4-chloro-1-(2-chloro-4-iodobenzyl)-2-methylimidazol-5-yl)-2-propenate (350 mg), 2-furylboronic acid (135 mg), potassium carbonate powder (321 mg) and N,N-dimethylformamide (3.5 ml) was stirred under a nitrogen atmosphere at 80° C. for 4 hr. The reaction mixture was allowed to cool to room temperature and water was added. The precipitate was collected by filtration. The precipitate was dissolved in chloroform, washed successively with saturated aqueous sodium hydrogencarbonate solution and saturated brine, and dried over magnesium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography (chloroform/ethyl acetate=10/1) to give methyl (E)-3-(4-chloro-1-(2-chloro-4-(2-furyl)benzyl)-2-methylimidazol-5-yl)-2-propenate (336 mg) as a pale-yellow powder.

1. temperatureto cool to room temperature
2. filtrationThe precipitate was collected by filtration
3. dissolutionThe precipitate was dissolved in chloroform
4. washwashed successively with saturated aqueous sodium hydrogencarbonate solution and saturated brine
5. dry with materialdried over magnesium sulfate
6. customThe solvent was evaporated
7. customthe residue was purified by silica gel column chromatography (chloroform/ethyl acetate=10/1)