反应详情

Under nitrogen bubbling, a mixure of 2-(3,4-dichlorophenyl)-3H-imidazo[4,5-b]pyridine-3-acetic acid (3.5 g, 0.011 mole) and 1,1'-carbonyldiimidazole (1.95 g, 0.011 mole) in 120 ml of tetrahydrofuran was stirred at room temperature for 31/2 hrs. Then, under nitrogen atmosphere, dipropylamine (2.43 g, 0.024 mole) was added at room temperature and the reaction mixture was heated at reflux for 6 hrs. The reaction mixture was filtered, and the filtrate was evaporated to dryness. The residue was treated with water and refrigerated. The solid was collected by filtration, washed with water, and dried under high vacuum at 50°-60° C. overnight. The solid was recrystallized from isopropyl alcohol-water, collected, washed with water, and dried under high vacuum at 50°-60° C. overnight. Two crops gave 1.9 g (43%) of crystals, mp 122°-123° C.

1. temperaturethe reaction mixture was heated
2. temperatureat reflux for 6 hrs
3. filtrationThe reaction mixture was filtered
4. customthe filtrate was evaporated to dryness
5. additionThe residue was treated with water
6. filtrationThe solid was collected by filtration
7. washwashed with water
8. customdried under high vacuum at 50°-60° C. overnight
9. customThe solid was recrystallized from isopropyl alcohol-water
10. customcollected
11. washwashed with water
12. customdried under high vacuum at 50°-60° C. overnight