反应详情

温度

70 °C

To a solution of 1.67 g of 3-hydroxy-2,2-dimethyl-1-propanesulfonamide in 30 ml of DMF was added 0.8 g of sodium hydride, followed by heating at 70° C. for an hour. The mixture to which 1.88 g of 6-chloroimidazo [1,2-b]pyridazine was added was heated for 4.5 hours. The reaction mixture was distilled to remove the solvent under reduced pressure and 50 ml of ice-water was added to the residue. The mixture was adjusted to pH 6.0 with 1N-hydrochloric acid and then extracted with tetrahydrofuran and ethyl acetate (1:1). The extract was dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The residue was subjected to a silica gel column chromatography, eluting with chloroform and methanol (20:1). The corresponding combined fractions were concentrated to obtain 1.56 g of the title compound.

1. temperaturewas heated for 4.5 hours
2. distillationThe reaction mixture was distilled
3. customto remove the solvent under reduced pressure and 50 ml of ice-water
4. additionwas added to the residue
5. extractionextracted with tetrahydrofuran and ethyl acetate (1:1)
6. dry with materialThe extract was dried over anhydrous magnesium sulfate
7. distillationdistilled under reduced pressure
8. customto remove the solvent
9. washeluting with chloroform and methanol (20:1)
10. concentrationThe corresponding combined fractions were concentrated