Hydrochloric Acid → N-{4-Methyl-3-[6-(pyridin-3-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]phenyl}-3-(pentafluoro-lambda6-sulphanyl)-5-(piperazin-1-yl)benzamide

Participants

Reaction Conditions

Reaction Steps

120 mg (0.42 mmol) of the compound of Example 6A and 179 mg (0.42 mmol) of the compound of Example 16A were reacted and worked up analogously to the procedure of Example 16. In this manner, 260 mg (89% of theory) of the Boc-protected intermediate tert-butyl 4-[3-({4-methyl-3-[6-(pyridin-3-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]phenyl}carbamoyl)-5-(pentafluoro-λ6-sulphanyl)-phenyl]piperazine-1-carboxylate were obtained. This compound was dissolved in 3 ml of 1,4-dioxane and 1 ml of methanol, 0.31 ml (1.24 mmol) of a 4 M solution of hydrogen chloride in 1,4-dioxane was added and the mixture was stirred at 80° C. for 1 h. The mixture was then concentrated under reduced pressure and the residue was purified by preparative HPLC (Method 18). The product fractions were concentrated and the residue was dissolved in ethyl acetate and washed successively with saturated potassium carbonate solution and saturated sodium chloride solution. The organic phase was dried over sodium sulphate, filtered and concentrated under reduced pressure. Drying of the residue gave 155 mg (62% of theory) of the title compound.

Provenance & Evidence