反应详情

To a solution of iodine (3.55 g, 14.0 mmol) in 100 mL absolute ethanol at room temperature was added silver sulfate (4.37 g, 14.0 mmol) and methyl 6-aminonicotinate (1.52 g, 10.0 mmol). After 42 hours the reaction was filtered to isolate a tan precipitate. The solid was heated with 20% MeOH/CHCl3 then cooled to room temperature, filtered, and rinsed with MeOH and CHCl3. The filtrate was evaporated, dissolved in hot MeOH, filtered to remove brownish impurities, and then crystallized from MeOH to give the title compound as a light tan solid (1.73 g, 62%).

1. filtrationAfter 42 hours the reaction was filtered
2. customto isolate a tan precipitate
3. filtrationfiltered
4. washrinsed with MeOH and CHCl3
5. customThe filtrate was evaporated
6. dissolutiondissolved in hot MeOH
7. filtrationfiltered
8. customto remove brownish impurities
9. customcrystallized from MeOH