Pamidronic Acid → Pamidronate disodium hydrate

HRID 1862081

Reaktionsgleichung

Reaktionsgleichung von HRID 1862081
[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]

Komponenten

9

Edukt 5

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

Produkt 1

HCID 16078998Pamidronate disodium hydrate

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-034065f4d7b54650938756b96dd24b9c
Quelldatensatz
uspto-grants-2003_03
Patentnummer
US06534674B2

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