Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229916Notes

Reaction equation

HRID 229916 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(O)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

5

Reactant 2

HCID 14798Sodium HydroxideHCID 60852Ibandronate

Product 1

HCID 23670359Ibandronate Sodium AnhydrousYield 93%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

A solution of sodium hydroxide (0.63 g) in water (12.5 ml) was added dropwise to a slurry of amorphous ibandronic acid (5 g) in ethanol (70 ml) at reflux temperature. Then the solution was cooled to room temperature and stirred for 72 hours to obtain a pH of 4.15. The precipitate was isolated by vacuum filtration, washed with ethanol (2×25 ml), and dried in a vacuum oven at 50° C. for 23 hours to obtain 4.97 g of ibandronate sodium crystal form QQ.

Workup

  1. temperatureat reflux temperature
  2. customto obtain a pH of 4.15
  3. customThe precipitate was isolated by vacuum filtration
  4. washwashed with ethanol (2×25 ml)
  5. customdried in a vacuum oven at 50° C. for 23 hours

Sources & evidence

ORD record
ord-8bca2ab968f44ce9ac47787a0bfea1cd
Source dataset
uspto-grants-2009_07
Patent number
US07563918B2

Reaction notes

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