反应详情

温度

120 °C

Phosphorus pentachloride (0.5 g) was added to methanesulfonic acid (2 ml), and the mixture was stirred at 120° C. for 1 hour to make a solution. To the solution were added 2,3-diamino-6-phenylpyridine (Compound of Reference Example 113) (0.2 g) and 3-methoxybenzoic acid (0.17 g), and the mixture was stirred at 120° C. for 1 hour. The reaction mixture was poured onto ice, neutralized with 8 N sodium hydroxide solution and extracted with ethyl acetate-tetrahydrofuran (3:1, v/v). The organic layer was washed with water and dried over MgSO4. The solvent was distilled off under reduced pressure, and the resulting crystals were collected by filtration to obtain 5-phenyl-2-(3-methoxyphenyl)-1H-imidazo[4,5-b]pyridine (0.18 g, 55%).

1. stirringthe mixture was stirred at 120° C. for 1 hour
2. additionThe reaction mixture was poured onto ice
3. extractionextracted with ethyl acetate-tetrahydrofuran (3:1
4. washThe organic layer was washed with water
5. dry with materialdried over MgSO4
6. distillationThe solvent was distilled off under reduced pressure
7. filtrationthe resulting crystals were collected by filtration