Acetone → Ibandronate Sodium Anhydrous

HRID 229903

Reaktionsgleichung

Reaktionsgleichung von HRID 229903
[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>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

5

Edukt 3

HCID 180AcetoneHCID 14798Sodium HydroxideHCID 60852Ibandronate

Produkt 1

HCID 23670359Ibandronate Sodium AnhydrousAusbeute 100,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of amorphous ibandronic acid (4.5 g) in water (11 ml) and sodium hydroxide (0.56 g, solid) was stirred at room temperature. The solution was added dropwise into acetone (100 ml). The resulting precipitate was stirred at room temperature for 16 hours. The precipitate was isolated by vacuum filtration, washed with acetone (2×10 ml), and dried in a vacuum oven at 50° C. for 24 hours to obtain 4.8 g of ibandronate sodium crystal form Q.

Aufarbeitung

  1. customThe precipitate was isolated by vacuum filtration
  2. washwashed with acetone (2×10 ml)
  3. customdried in a vacuum oven at 50° C. for 24 hours

Quellen und Nachweise

ORD-Eintrag
ord-6a1b82f6e5fa454ca04159f11d79f476
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07563918B2

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