反应详情

温度

80 °C

1,3-Di(2-pyridyl)propane-1,3-dione (1.17 g, 5.15 mmol) was dissolved in acetic acid (20 mL), and bromine (856 mg, 5.35 mmol) was added thereto, followed by stirring at 80° C. for 1 hour. The reaction mixture was concentrated under reduced pressure, and the resulting residue was suspended in ethanol (30 mL), and triethylamine (0.750 mL, 5.38 mmol) and thiourea (416 mg, 5.47 mmol) were added thereto, followed by stirring under heating and reflux for 30 minutes. Aqueous saturated sodium hydrogencarbonate solution was added to the reaction mixture, followed by extraction with chloroform. The solvent was distilled away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (chloroform:methanol=9:1) to afford the entitled Compound 630 (739 mg, 51%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. stirringby stirring
3. temperatureunder heating
4. temperaturereflux for 30 minutes
5. extractionfollowed by extraction with chloroform
6. distillationThe solvent was distilled away under reduced pressure
7. customthe resulting residue was purified through silica gel column chromatography (chloroform:methanol=9:1)