HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Hydroxide → Ibandronate Sodium Anhydrous
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Ibandronate | HCID 60852 | — |
| Lösungsmittel | Propan-2-ol--water (1/1) | HCID 21889133 | — |
| Produkt | Ibandronate Sodium Anhydrous | HCID 23670359 | 80,5% |
Reaktionsschritte
A solution of sodium hydroxide (0.63 g) in water:IPA (40:60 v/v, 12 ml) was added dropwise to a solution of amorphous ibandronic acid (5 g) in water:IPA (40:60 v/v, 71 ml) at reflux temperature. The reaction mixture was heated at reflux temperature for an additional 4 hours to obtain a pH of 4.0-4.12. Then the reaction mixture was cooled to room temperature and stirred for 16 hours. Further cooling was performed using an ice-bath. The precipitate was filtered, washed with IPA (2×25 ml), and dried in a vacuum oven at 50° C. for 24 hours to give 4.3 g of ibandronate sodium crystal form F.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07563918B2 |
| Quelldatensatz | uspto-grants-2009_07 |
| ORD ID | ord-dc4f3cca29fe420f9d5e360256505234 |
| Quellennotiz | uspto-grants-2009_07 |