反应详情

A mixture of 7-iodo-1-phenyl-5-trifluoromethylbenzimidazole (7.38 g, 19 mmol), 3-acetylphenyl boronic acid (4.67 g, 28.5 mmol), 1,3-propanediol (6.8 ml, 95 mmol), potassium carbonate (13.1 g, 95 mmol) and bis(triphenylphosphin)palladium dichloride (200 mg, 0.28 mmol) in a mixture of dimethoxyethane (60 ml) and water (30 ml) was stirred at reflux in a nitrogen atmosphere for 1 hour. The cooled reaction mixture was filtered through a pad of Celite and the filter was rinsed with ethyl acetate. The organic layer was collected, dried over magnesium sulphate and concentrated under reduced pressure. The title product precipitated upon addition of diethyl ether to the concentrate (6.17 g, 85%) m/z, 381.1 (M+H)+.

1. temperatureat reflux in a nitrogen atmosphere for 1 hour
2. customThe cooled reaction mixture
3. filtrationwas filtered through a pad of Celite
4. washthe filter was rinsed with ethyl acetate
5. customThe organic layer was collected
6. dry with materialdried over magnesium sulphate
7. concentrationconcentrated under reduced pressure
8. customThe title product precipitated upon addition of diethyl ether to the
9. concentrationconcentrate (6.17 g, 85%) m/z, 381.1 (M+H)+