反应详情

温度

80 °C

Compound 610 (100 mg, 0.359 mmol) was dissolved in pyridine (3 mL), and 6-chloroisonicotinoyl chloride (560 mg, 3.18 mmol) and DMAP (4.40 mg, 0.0360 mmol) were added thereto, followed by stirring at 80° C. for 3 hours. The reaction mixture was concentrated under reduced pressure, and the resulting residue was poured into a saturated aqueous solution of sodium hydrogencarbonate, and the precipitated solid was collected by filtration. The resulting solid was purified through silica gel column chromatography (hexane:ethyl acetate=3:1), followed by recrystallizing from a mixed solvent of ethanol and water to afford the entitled Compound 616 (54.5 mg, 36%) as a white solid.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionthe resulting residue was poured into a saturated aqueous solution of sodium hydrogencarbonate
3. filtrationthe precipitated solid was collected by filtration
4. customThe resulting solid was purified through silica gel column chromatography (hexane:ethyl acetate=3:1)
5. customby recrystallizing from a mixed solvent of ethanol and water