Acetone → Ibandronate Sodium Anhydrous

HRID 229903

Reaction equation

HRID 229903 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(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]

Participants

5

Reactant 3

HCID 180AcetoneHCID 14798Sodium HydroxideHCID 60852Ibandronate

Product 1

HCID 23670359Ibandronate Sodium AnhydrousYield 100.5%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-6a1b82f6e5fa454ca04159f11d79f476
Source dataset
uspto-grants-2009_07
Patent number
US07563918B2

Linked notes

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