Hydrochloric Acid → 2-{5-Chloro-2-[3-(4-methyl-piperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophene-6-carboxylic acid tri-hydrochloride

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Reaction Steps

Aqueous LiOH solution (2.0 M, 2.8 mL) is added to a stirred suspension of 2-{5-chloro-2-[3-(4-methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophene-6-carboxylic acid methyl ester (0.840 g, 1.80 mmol) in MeOH (20 mL)/THF (20 mL)/H2O (6 mL), the resultant mixture is heated at 70° C. for 4.5 hours. While heating the solution, 5.0 N HCl (3.4 mL) is added in one portion then the solution is allowed to cool to ambient temperature to from a suspension. After filtration, the solid is dried in a vacuum oven at 60° C. for 4 hours to give the title compound (0.64 g, 67% yield). ES+(m/z) 446 (35Cl) and 448 (37Cl) [M+H].

Provenance & Evidence