Sodium Hydroxide → Ibandronate Sodium Anhydrous

Participants

Reaction Steps

A solution of sodium hydroxide (0.63 g) in a mixture of water:acetonitrile (60:40 v/v, 19 ml) was added dropwise to a solution of amorphous ibandronic acid (5 g) in water:acetonitrile (60:40 v/v, 106 ml) at reflux temperature. The solution was heated at reflux temperature for an additional 1 hour. Then the reaction mixture was cooled to room temperature. Further cooling was performed using an ice-bath. Seeding was done, and the reaction mixture was stirred at 10° C. for 16 hours. The precipitate was isolated by vacuum filtration, washed with acetonitrile (2×10 ml), and dried in a vacuum oven at 50° C. for 23 hours to obtain 1.0 g of ibandronate sodium crystal form Q.

Provenance & Evidence