Sodium Hydroxide → Ibandronate Sodium Anhydrous

Participants

Reaction Steps

A slurry of amorphous ibandronic acid (5 g) in methanol (50 ml) was heated to reflux temperature. Sodium hydroxide (0.63 g, solid) was added, and the reaction mixture was stirred at reflux temperature for an additional 4 hours to obtain a pH of 4.0. Then the reaction mixture was cooled to room temperature. Further cooling was performed using an ice-bath. The white solid was filtered, washed with methanol (2×25 ml), and dried in a vacuum oven at 50° C. for 19 hours to give 4.7 g of ibandronate sodium crystal form Q3.

Provenance & Evidence