Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229902

Reaktionsgleichung

Reaktionsgleichung von HRID 229902
[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]>C(O)C>[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 102,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A slurry of amorphous ibandronic acid (5 g) in ethanol (50 ml) was heated to reflux temperature. Sodium hydroxide (0.63 g, solid) was added, and the reaction mixture was stirred at reflux temperature for an additional 4 hours to obtain a pH of 3.5. Then the reaction mixture was cooled to room temperature. Further cooling was performed using an ice-bath. The white solid was filtered, washed with ethanol (2×25 ml), and dried in a vacuum oven at 50° C. for 20 hours to give 5.5 g of ibandronate sodium crystal form Q.

Aufarbeitung

  1. temperatureto reflux temperature
  2. temperatureat reflux temperature for an additional 4 hours
  3. customto obtain a pH of 3.5
  4. temperatureFurther cooling
  5. filtrationThe white solid was filtered
  6. washwashed with ethanol (2×25 ml)
  7. customdried in a vacuum oven at 50° C. for 20 hours

Quellen und Nachweise

ORD-Eintrag
ord-4ee7c6e7224445b38017c457ddaab4c7
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07563918B2

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