反应详情

温度

90 °C

(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-imidazo[1,2-a]pyridin-6-yl-methanone (Stage 292.2, 4.0 g, 13.44 mmol) was suspended in dioxane (400 mL) and it was heated at 90° C. When all the material was in solution, it was cooled down to 50° C. and the 3 M methylmagnesium bromide solution (28.8 mL, 40.3 mmol) was added. It was refluxed for 2 h. Then it was cooled down to rt and the precipitate formed was filtered off. It was taken up with EtOAc/MeOH (9:1) and washed with saturated NaHCO3 solution and brine. The organic layer was dried over Na2SO4, filtered and concentrated to give the title compound as a brown solid (tR 0.3 min (conditions 2), MH+=314)

1. temperaturewas cooled down to 50° C.
2. temperatureIt was refluxed for 2 h
3. temperatureThen it was cooled down to rt
4. customthe precipitate formed
5. filtrationwas filtered off
6. washwashed with saturated NaHCO3 solution and brine
7. dry with materialThe organic layer was dried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated