反应详情

Palladium tetrakis(triphenylphosphine) (107 mg, 0.09 mmol) was added to a degassed, ambient temperature solution of 2-[(4-bromophenyl)acetyl]-4-(2,2-dimethylpropyl)-N,N-dimethyl-1H-imidazole-1-sulfonamide (intermediate 7) (410 mg, 0.9 mmol), 2-bromo-5-fluoropyridine (163 mg, 0.9 mmol) and hexamethylditin (304 mg, 0.9 mmol) in 1,4-dioxane (20 mL). After stirring at reflux overnight, the reaction mixture was diluted with water and extracted with ethyl acetate and methylene chloride. The combined organic extracts were dried (magnesium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-50% ethyl acetate/hexane afforded 4-(2,2-dimethylbutyl)-2-{[4-(5-fluoropyridin-2-yl)phenyl]acetyl}-N,N-dimethyl-1H-imidazole-1-sulfonamide.

1. temperatureat reflux overnight
2. extractionextracted with ethyl acetate and methylene chloride
3. dry with materialThe combined organic extracts were dried (magnesium sulfate)
4. concentrationconcentrated in vacuo