反应详情

To a solution of 3″-fluoro-3,2′:3′,4″-terpyridine-5′,6′-diamine (Intermediate 1, 158 mg, 0.56 mmol) in THF (5 mL) Et3N (156 μL, 1.12 mmol) and carbonyldiimidazole (182 mg, 1.12 mmol) were added sequentially. The reaction mixture was heated to reflux for 4 h and then the solvent was removed under reduced pressure. Flash chromatography of the resulting crude oil (CH2Cl2/EtOH/aq NH3 60:8:1 to 40:8:1) followed by reverse phase chromatography (0% CH3CN in H2O to 25% CH3CN in H2O) gave the title compound as a white solid (29 mg, 17%).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 4 h
3. customthe solvent was removed under reduced pressure