Isopropanol → Ibandronate Sodium Anhydrous

HRID 229900

Reaction equation

[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]

Participants

Conditions

Temperature: 0 °C

Procedure

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.

Workup

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

Sources & evidence

ORD record: ord-df61eb585e5741eda33bb880dec71106
Source dataset: uspto-grants-2009_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07563918B2

Linked notes

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