反应详情

A solution of sodium hydroxide (1.4 g) in a mixture of water (X % v/v)/Methanol (Y % v/v, 10 volumes per grams of ZLD-Ac form I) (15 ml) was added drop-wise to a suspension of Zoledronic acid form I (5.0 g) in a mixture of water (X % v/v)/Methanol (Y % v/v, 10 volumes per grams of ZLD-Ac) (85 ml) at reflux temperature. The reaction mixture was heated at reflux temperature for additional 16 hours. Then the reaction mixture was cooled to room temperature. Further cooling was performed using an ice-bath. The precipitate was then filtered, washed and dried in a vacuum oven at 50° C. for 24 hours to give Zoledronate disodium crystal form V. Purity by HPLC 99.95%.

1. additionwas added drop-wise
2. temperatureat reflux temperature
3. temperatureThe reaction mixture was heated
4. temperatureat reflux temperature for additional 16 hours
5. temperatureFurther cooling
6. filtrationThe precipitate was then filtered
7. washwashed
8. customdried in a vacuum oven at 50° C. for 24 hours