Methanesulfonic Acid → HCID 131728801, compound

Participants

Reaction Steps

A solution of 1.53 g (15.93 mmol) of methanesulfonic acid in 15 mL of ethyl acetate was added dropwise to a solution of 10.0 g (15.93 mmol) of ethyl 3-[(2-{[4-(hexyloxycarbonylaminoiminomethyl)phenylamino]methyl}-1-methyl-1H-benzimidazole-5-carbonyl)pyridin-2-ylamino]propionate base (prepared as described in WO 98/37075) in 16.5 mL of 90% aqueous ethanol and 40 mL of ethyl acetate, with stirring, at 35° C. to 40° C. After a few minutes, the product began to crystallize out and was diluted with 30 mL of ethyl acetate. It was stirred for another 30 minutes at 35° C. to 40° C. and for a further 30 minutes at ambient (room) temperature, then the precipitate was suction filtered, washed with approximately 20 mL of ethyl acetate, and dried at 40° C. in the circulating air drying cupboard.

Provenance & Evidence