Sodium Bicarbonate → HCID 178511751, compound

Participants

Reaction Conditions

Reaction Steps

Trovafloxacin mesylate, (75 g) was stirred with demineralised water (375 mL). The crystal slurry was heated to about 50° C. and the slurry adjusted to a pH of about 8.0 by addition of saturated sodium bicarbonate solution. The slurry was held at about 50° C. for 30 minutes, allowed to cool to about 25° C. and stirred at this temperature for 30 minutes. Crystals were isolated by filtration and washed with demineralised water (100 mL). The wet crystals were suspended in demineralised water (375 mL) and stirred for 1 hour at about 50° C., then cooled to about 20° C. and stirred at this temperature for about 1 hour. The crystalline product was filtered from the mother liquor and washed with demineralised water (about 100 mL). The wet crystals were stirred with ethyl acetate (1125 mL) and the resultant slurry heated to reflux and the water azeotropically removed. The essentially anhydrous slurry was cooled to about 25° C., the crystals were isolated by filtration and dried under vacuum at 40° C. until all the solvent had been removed to provide the title product. Yield 60.9 g, 94%.

Provenance & Evidence