反应详情

温度

135 °C

To a solution of methyl 5″-chloro-2,2′:5′,3″-terpyridine-3′-carboxylate (12-3, 3.05 g, 9.36 mmol, 1.0 equiv) in THF/methanol (22 mL/4.5 mL) was added 10 N sodium hydroxide (1.124 mL, 11.2 mmol, 1.2 equiv) and the system was heated to 135° C. for 15 minutes in a microwave reactor. The reaction mixture was cooled, concentrated, and azeotroped with ethyl acetate (2×100 mL) and toluene (3×100 mL) to afford the desired product (12-4) as a white solid. ESI+MS [M+H]+ C16H10ClN3O2 calc'd 312.0. found 311.9.

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated
3. customazeotroped with ethyl acetate (2×100 mL) and toluene (3×100 mL)