Methanesulfonic Acid → Methanesulfonic Acid

Participants

Reaction Conditions

Reaction Steps

To a 25-mL 3-neck flask under an inert nitrogen atmosphere, 3 mL of isopropanol (IPA) was charged. A slurry was prepared by adding 225 mg amorphous free base of Compound 1 to the flask. The slurry was warmed to a temperature of 45° C. Methanesulfonic acid hydrate (98.0 mg) was then added to the slurry. The slurry was stirred at 45° C. for one hour, then cooled to 22° C. to produce a thick crystalline slurry. The slurry was filtered and washed with IPA (2×1 mL). Excess IPA was removed from the crystalline cake by drying at 55° C. for more than two hours to achieve a constant weight. Crystalline mesylate (methanesulfonic acid) salt of Compound 1 (180 mg) was isolated. It was determined that the crystalline mesylate salt was unstable at 5° C.

Provenance & Evidence