Hydrochloric Acid → HCID 56645180, compound

Participants

Reaction Steps

210 mg Crude (1-{4-[3-(3-carbamoyl-phenyl)-2-methyl-7-phenyl-imidazo[1,2-b]pyridazin-6-yl]-phenyl}-cyclobutyl)-carbamic acid tert-butyl ester, intermediate example Int-4-0, were stirred with 15 mL 4M hydrogen chloride in dioxane over night at room temperature. The solvent was evaporated and the residue was dissolved in methanol/dichloromethane. Methyl-tert.butylether was added until the product precipitated. The reaction mixture was stirred for one hour and the precipitate was sucked off. The crystals were dissolved in methanol and given on a ForaPak Rxn CX column. The column was washed with 100 mL methanol and the product was eluted with methanol/NH3. After evaporation of the solvents the residue was purified by HPLC to yield 39.3 mg of the title compound.

Provenance & Evidence