反应详情

温度

80 °C

Under a nitrogen stream, a solution of n-propylzinc bromide in tetrahydrofuran (0.5 M, 7.98 ml, 3.99 mmol) was diluted with toluene (5.0 ml), and 2,6-dichloroimidazo[1,2-b]pyridazine (0.50 g, 2.66 mmol) and bis(triphenylphosphine)palladium(II) dichloride (0.19 g, 0.27 mmol) were added thereto, and the reaction mixture was stirred for 2 hours at 80° C. After cooling, to the reaction mixture was added cold water (50 ml), acidified with dilute hydrochloric acid, extracted with ethyl acetate, and the extracts were washed with dilute hydrochloric acid, a saturated saline, an aqueous saturated sodium bicarbonate solution and a saturated saline in this order. The resulting organic layer was dried over anhydrous magnesium sulfate, filtrated and concentrated. The concentrated residue was purified by silica gel column chromatography (ethyl acetate:hexane=3:7) to give the title compound as white crystals. The yield was 0.31 g (59.6%).

1. additionwere added
2. temperatureAfter cooling, to the reaction mixture
3. extractionextracted with ethyl acetate
4. washthe extracts were washed with dilute hydrochloric acid
5. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
6. filtrationfiltrated
7. concentrationconcentrated
8. customThe concentrated residue was purified by silica gel column chromatography (ethyl acetate:hexane=3:7)