Sodium Hydroxide → Zoledronate disodium tetrahydrate

Participants

Reaction Conditions

Reaction Steps

A 0.5 liter reactor equipped with a mechanical stirrer, a thermometer, a reflux condenser and a dropping funnel, was loaded with Zoledronic acid form I (20.0 g) and water (260 ml). The suspension was heated to reflux temperature (92° C.) to obtain a clear solution. A 40% aqueous solution of Sodium hydroxide (13.8 g) was added drop-wise. The solution was then cooled to 25° C. and was stirred at this temperature for about 16 hours. The solution was then concentrated to half of its volume to obtain a precipitate. After stirring at 0° C. for 72 hours, the white precipitate was filtered and dried in a vacuum oven at 50° C. for 23 hours to obtain 10.4 g of Zoledronate disodium crystal form XIX.

Provenance & Evidence