反应详情

Under nitrogen atmosphere, the 2-(4-chlorophenyl)-3H-imidazo[4,5-b]pyridine (5.0 g, 0.022 mole) was added to a suspension of sodium hydride (0.96 g of 60% in oil, 0.024 mole, washed once with hexanes) in dimethylformamide (100 ml). The mixture was heated at 70°-85° C. for 1.5 hr before adding the α-bromoacetophenone (4.38 g, 0.022 mole) at room temperature. The reaction mixture was stirred at room temperature overnight, then poured into water. The precipitate was collected by filtration, washed with water, and dried under high vacuum. A sample was dissolved in isopropyl alcohol, then concentrated to initiate crystallization. The crystals were collected by filtration, washed with isopropyl alcohol, and dried under high vacuum at 70° C. over a weekend to give 1.5 g (20%) of title compound, mp. 262°-263° C.

1. washwashed once with hexanes) in dimethylformamide (100 ml)
2. temperatureThe mixture was heated at 70°-85° C. for 1.5 hr
3. filtrationThe precipitate was collected by filtration
4. washwashed with water
5. customdried under high vacuum
6. dissolutionA sample was dissolved in isopropyl alcohol
7. concentrationconcentrated
8. customcrystallization
9. filtrationThe crystals were collected by filtration
10. washwashed with isopropyl alcohol
11. customdried under high vacuum at 70° C. over a weekend