反应详情

温度

70 °C

To a solution of 3.5 g of 3-hydroxy-2,2-dimethyl-1-propanesulfonamide in 30 ml of DMF was added by portions 0.85 g of sodium hydride (60%, in oil)with stirring. To the mixture were added 3.18 g of 6-chloroimidazo[1,2-b]pyridazine and then 0.85 g of sodium hydride. The reaction solution was heated at 70° C. for 1.5 hours and then at 100° C. for an hour with stirring, and concentrated under reduced pressure. The residue was added into 100 ml of ice-water, extracted with ethyl acetate and tetrahydrofuran (1:1) (100 ml×4), dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The residue was recrystallized from ethanol to obtain 5.18 g of the title compound.

1. stirringat 100° C. for an hour with stirring
2. concentrationconcentrated under reduced pressure
3. additionThe residue was added into 100 ml of ice-water
4. extractionextracted with ethyl acetate and tetrahydrofuran (1:1) (100 ml×4)
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationdistilled under reduced pressure
7. customto remove the solvent
8. customThe residue was recrystallized from ethanol