反应详情

1.12 g of 60% oily sodium hydride was suspended in 25 ml of dimethylformamide. To this suspension, 1.51 g of 3-hydroxy-2,2-dimethyl-1-propanesulfonamide was added, followed by stirring at room temperature (15° to 20° C.) under reduced pressure for i hour. To this mixture was added 1.51 g of 6-chloro-7-methylimidazo[1,2-b]pyridazine, followed by stirring at 60° C. for 2 hours. After dimethylformamide was distilled off underreduced pressure, ice water was added to the residue, which was subsequently adjusted to pH 6 by the addition of 5 N hydrochloric acid andthen extracted with tetrahydrofuran. The extract was washed with 20 ml of saturated saline and then dried over magnesium sulfate. After the solvent was distilled off under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with dichloromethane-ethyl acetate-methanol (5:5:1). The fraction containing the desired product was concentrated and recrystallized by the addition of ethyl ether-ethyl acetate (5:1). The resulting crystal was collected by filtration, to yield0.522 g of the title compound.

1. stirringby stirring at 60° C. for 2 hours
2. distillationAfter dimethylformamide was distilled off underreduced pressure, ice water
3. additionwas added to the residue, which
4. additionwas subsequently adjusted to pH 6 by the addition of 5 N hydrochloric acid
5. extractionandthen extracted with tetrahydrofuran
6. washThe extract was washed with 20 ml of saturated saline
7. dry with materialdried over magnesium sulfate
8. distillationAfter the solvent was distilled off under reduced pressure
9. washeluted with dichloromethane-ethyl acetate-methanol (5:5:1)
10. additionThe fraction containing the desired product
11. concentrationwas concentrated
12. customrecrystallized by the addition of ethyl ether-ethyl acetate (5:1)
13. filtrationThe resulting crystal was collected by filtration, to yield0.522 g of the title compound