Pamidronic Acid → Pamidronate disodium hydrate

HRID 1862081

반응식

HRID 1862081 반응식
[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]

참가 물질

9

반응물 5

HCID 4674Pamidronic Acid2회HCID 73351Pamidronate Disodium AnhydrousHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 10942334Sodium Methoxide

생성물 1

HCID 16078998Pamidronate disodium hydrate

시약·촉매·용매 3

HCID 702Ethanol용매HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-034065f4d7b54650938756b96dd24b9c
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06534674B2

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