反应详情

A slurry of amorphous ibandronic acid (4.6 g) in acetone (96 ml) was heated to reflux temperature. Sodium hydroxide (0.58 g, solid) was added, and the reaction mixture was stirred at reflux temperature for an additional 10 hours to obtain a pH of 3.35. Then the reaction mixture was cooled to room temperature. Further cooling was performed using an ice-bath. The white solid was filtered, washed with acetone (2×25 ml), and dried in a vacuum oven at 50° C. for 21 hours to give 4.5 g of ibandronate sodium crystal form Q.

1. temperatureto reflux temperature
2. temperatureat reflux temperature for an additional 10 hours
3. customto obtain a pH of 3.35
4. temperatureFurther cooling
5. filtrationThe white solid was filtered
6. washwashed with acetone (2×25 ml)
7. customdried in a vacuum oven at 50° C. for 21 hours