反应详情

温度

120 °C

A mixture of 6-chloroimidazo[1,2-b]pyridazine (1536 mg, 10.0 mmol), methyl 3-hydroxybenzoate (1978 mg, 13.0 mmol), potassium carbonate (4146 mg, 30.0 mmol) and N-methylpyrrolidone (10 mL) was stirred at 120° C. for 18 hr. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and concentrated under reduced pressure. The residue was purified by NH silica gel column chromatography (hexane/ethyl acetate=90/10→20/80). The objective fraction was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=60/40→0/100) and precipitated from diisopropyl ether to give the title compound (1722 mg, 6.4 mmol, yield 64%) as a white solid.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with water
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by NH silica gel column chromatography (hexane/ethyl acetate=90/10→20/80)
5. concentrationThe objective fraction was concentrated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate=60/40→0/100)
7. customprecipitated from diisopropyl ether