Sodium Hydroxide → Ibandronate Sodium Anhydrous

Participants

Reaction Steps

A solution of sodium hydroxide (0.57 g) in water:acetone (40:60 v/v, 11.4 ml) was added dropwise to a solution of amorphous ibandronic acid (4.5 g) in water:acetone (40:60 v/v, 64.4 ml) at reflux temperature. The reaction mixture was heated at reflux temperature for an additional 2 hours to obtain a pH of 4.5. Then the solution was cooled to room temperature. Further cooling was performed using an ice-bath. The precipitate was isolated by vacuum filtration, washed with acetone (2×15 ml), and dried in a vacuum oven at 50° C. for 21 hours to obtain 3.9 g of ibandronate sodium crystal form QQ.

Provenance & Evidence