反应详情

6-(1-Methyl-1H-pyrazol-4-yl)-3-(3-vinyl-imidazo[1,2-a]pyridin-6-ylmethyl)-imidazo[1,2-b]pyridazine (Example 299, 49 mg, 0.138 mmol) was dissolved in dioxane (0.69 mL) and water (0.69 mL) then KMnO4 (21.8 mg, 0.138 mmol) and 2.5 M NaOH solution (0.165 mL, 0.414 mmol) were added. The RM was stirred at rt for 3 h. It was then filtered through Celite and the solvent was removed. The residue was purified by preparative HPLC with acetonitrile and water (+0.1% TFA). The fractions were joined and were lyophilized. The residue was dissolved in MeOH and it was passed through an SPE cartridge of HCO3− to remove the TFA salt. The filtrate was evaporated and the residue was triturated with pentane. The precipitate was filtered off and dried to afford the title compound as a white solid (tR 0.3 min (conditions 2), MH+=390).

1. filtrationIt was then filtered through Celite
2. customthe solvent was removed
3. customThe residue was purified by preparative HPLC with acetonitrile and water (+0.1% TFA)
4. dissolutionThe residue was dissolved in MeOH
5. customto remove the TFA salt
6. customThe filtrate was evaporated
7. customthe residue was triturated with pentane
8. filtrationThe precipitate was filtered off
9. customdried