Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229926Notes

Reaction equation

HRID 229926 reaction equation
[OH-].[Na+:2].[CH3:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]([CH2:10][CH2:11][C:12]([P:18]([OH:21])([OH:20])=[O:19])([P:14]([OH:17])([OH:16])=[O:15])[OH:13])[CH3:9]>O.C(#N)C>[CH3:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]([CH2:10][CH2:11][C:12]([P:18]([O-:21])([OH:20])=[O:19])([P:14]([OH:17])([OH:16])=[O:15])[OH:13])[CH3:9].[Na+:2]

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 60852Ibandronate

Product 1

HCID 23670359Ibandronate Sodium AnhydrousYield 121.6%

Reagents, catalysts & solvents 1

HCID 18373917Acetonitrile--water (1/1)Solvent2×

Procedure

A solution of sodium hydroxide (0.55 g) in water:acetonitrile (80:20 v/v, 33 ml) was added dropwise to a solution of amorphous ibandronic acid (4 g) in water:acetonitrile (80:20 v/v, 187 ml) at reflux temperature. Then the reaction mixture was cooled to room temperature. The clear solution was evaporated until dry to obtain 5.2 g of amorphous ibandronate sodium.

Workup

  1. temperatureat reflux temperature
  2. customThe clear solution was evaporated
  3. customuntil dry

Sources & evidence

ORD record
ord-35c373a617964823b53de7e61fd11913
Source dataset
uspto-grants-2009_07
Patent number
US07563918B2

Reaction notes

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