Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229915Notes

Reaction equation

HRID 229915 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]>C(O)C>[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

4

Reactant 2

HCID 14798Sodium HydroxideHCID 60852Ibandronate

Product 1

HCID 23670359Ibandronate Sodium AnhydrousYield 87.9%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
55 °C

Procedure

Amorphous ibandronic acid (5 g) was added to a solution of solid sodium hydroxide (0.6 g) dissolved in 93% ethanol (100 ml) at 55° C. The obtained slurry was stirred at 55° C. for 3 hours. Then the slurry was cooled to room temperature. The precipitate was isolated by vacuum filtration, washed with 93% ethanol (3×25 ml), and dried in a vacuum oven at 50° C. for 24 hours to give 4.5 g of ibandronate sodium crystal form QQ.

Workup

  1. temperatureThen the slurry was cooled to room temperature
  2. customThe precipitate was isolated by vacuum filtration
  3. washwashed with 93% ethanol (3×25 ml)
  4. customdried in a vacuum oven at 50° C. for 24 hours

Sources & evidence

ORD record
ord-116caa0774df467993201593a028102f
Source dataset
uspto-grants-2009_07
Patent number
US07563918B2

Reaction notes

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