Isopropanol → Ibandronate Sodium Anhydrous

HRID 229900

Reaktionsgleichung

Reaktionsgleichung von HRID 229900
[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(O)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

5

Edukt 3

HCID 3776IsopropanolHCID 14798Sodium HydroxideHCID 60852Ibandronate

Produkt 1

HCID 23670359Ibandronate Sodium AnhydrousAusbeute 93,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of amorphous ibandronic acid (2.7 g) in water (25 ml) and sodium hydroxide (0.34 g, solid) was stirred at 70° C. The solution was poured into cold IPA (500 ml). The resulting precipitate was stirred at 0° C. for 16 hours. The precipitate was isolated by vacuum filtration and dried in a vacuum oven at 50° C. for 24 hours to obtain 2.7 g of ibandronate sodium crystal form K3. Form K3 can exhibit a weight loss of about 7% to about 8% in TGA.

Aufarbeitung

  1. customThe precipitate was isolated by vacuum filtration
  2. customdried in a vacuum oven at 50° C. for 24 hours

Quellen und Nachweise

ORD-Eintrag
ord-df61eb585e5741eda33bb880dec71106
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07563918B2

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