Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229901

Reaktionsgleichung

Reaktionsgleichung von HRID 229901
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:8][CH2:9][C:10]([P:16]([OH:19])([OH:18])=[O:17])([P:12]([OH:15])([OH:14])=[O:13])[OH:11])[CH3:7].[OH-].[Na+:21]>CC(C)=O>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:8][CH2:9][C:10]([P:16]([O-:19])([OH:18])=[O:17])([P:12]([OH:15])([OH:14])=[O:13])[OH:11])[CH3:7].[Na+:21]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 60852Ibandronate

Produkt 1

HCID 23670359Ibandronate Sodium AnhydrousAusbeute 91,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-96bce559a94448e1b859bceddf2c41fe
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07563918B2

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