Pamidronic Acid → Pamidronate disodium hydrate

HRID 1862081Notes

Reaction equation

HRID 1862081 reaction equation
[CH2:1]([C:4]([P:10]([O-:13])([OH:12])=[O:11])([P:6]([O-:9])([OH:8])=[O:7])[OH:5])[CH2:2][NH2:3].[Na+:14].[Na+].C(C(P(O)(O)=O)(P(O)(O)=O)[OH:20])CN.[Na].C[O-].[Na+].[O-]CC.[Na+]>CO.C(O)C.O>[CH2:1]([C:4]([P:10]([O-:13])([OH:12])=[O:11])([P:6]([O-:8])([OH:9])=[O:7])[OH:5])[CH2:2][NH2:3].[OH2:20].[Na+:14].[Na+:14]

Participants

9

Reactant 5

HCID 4674Pamidronic Acid2×HCID 73351Pamidronate Disodium AnhydrousHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 10942334Sodium Methoxide

Product 1

HCID 16078998Pamidronate disodium hydrate

Reagents, catalysts & solvents 3

HCID 702EthanolSolventHCID 887MethanolSolventHCID 962WaterSolvent

Procedure

In the process for preparing crystalline disodium pamidronate from the reaction solution of neutralization of pamidronic acid with an organic sodium compound according to the second method, it is characterized to be included the process which pamidronic acid is neutralized with sodium methoxide or sodium ethoxide in absolute methanol or absolute ethanol under refluxing: the salt produced from neutralization is dissolved in water and the insoluble materials produced are filtered: the filtrate is allowed to stand at room temperature to induce crystallization: the resulting solution is slowly cooled and filtered to obtain the crystals: and then the resulting crystals are dried at temperature of 75˜85° C. under normal pressure to obtain the crystalline disodium pamidronate hydrate.

Workup

  1. temperatureunder refluxing
  2. customthe salt produced from neutralization
  3. customthe insoluble materials produced
  4. filtrationare filtered
  5. customto stand at room temperature
  6. customcrystallization
  7. temperaturethe resulting solution is slowly cooled
  8. filtrationfiltered
  9. customto obtain the crystals
  10. customthe resulting crystals are dried at temperature of 75˜85° C. under normal pressure

Sources & evidence

ORD record
ord-034065f4d7b54650938756b96dd24b9c
Source dataset
uspto-grants-2003_03
Patent number
US06534674B2

Reaction notes

Loading…