反应详情

A mixture of 2-(5-methyl-2-thienyl)-3H-imidazo[4,5-b]pyridine-3-acetic acid (5.0 g, 0.0183 mole) and 1,1'-carbonyldiimidazole (2.97 g, 0.0183 mole) was stirred at room temperature in dry tetrahydrofuran (100 ml) for 2.5 hours with a stream of nitrogen bubbling through it. The reaction mixture was cooled in a dry ice/acetone bath, and liquid ammonia (50 ml) was added. The mixture was allowed to warm to room temperature and was stirred for 2 days under nitrogen atmosphere. The solvents were removed under reduced pressure and the resulting solid was triturated in water, collected by filtration, rinsed twice with water, twice with a 5% potassium hydroxide solution and twice again with water. The solid was recrystallized from hot methanol and dried under high vacuum at 40° C. to give 2.82 g (56%) of title compound, mp >250° C.

1. temperatureThe reaction mixture was cooled in a dry ice/acetone bath
2. customThe solvents were removed under reduced pressure
3. customthe resulting solid was triturated in water
4. filtrationcollected by filtration
5. washrinsed twice with water, twice with a 5% potassium hydroxide solution and twice again with water
6. customThe solid was recrystallized from hot methanol
7. customdried under high vacuum at 40° C.