Sodium Hydroxide → 827573-11-5

HRID 730614Notes

Reaction equation

HRID 730614 reaction equation
[OH-].[Na+:2].[CH:3]1[N:7]=[CH:6][N:5]([CH2:8][C:9]([P:15]([OH:18])([OH:17])=[O:16])([P:11]([OH:14])([OH:13])=[O:12])[OH:10])[CH:4]=1>O.CC(O)C.CO.C(O)C.CN(C=O)C>[CH:3]1[N:7]=[CH:6][N:5]([CH2:8][C:9]([P:11]([O-:14])([O-:13])=[O:12])([P:15]([O-:17])([OH:18])=[O:16])[OH:10])[CH:4]=1.[Na+:2].[Na+:2].[Na+:2]

Participants

8

Reactant 2

HCID 14798Sodium HydroxideHCID 68740Zoledronic Acid

Product 1

HCID 70695671827573-11-5

Reagents, catalysts & solvents 5

HCID 702EthanolSolvent2×HCID 887MethanolSolvent2×HCID 962WaterSolvent2×HCID 3776IsopropanolSolventHCID 6228DimethylformamideSolvent2×

Procedure

A solution of sodium hydroxide (1.4 g) in a mixture of water (50% v/v)/Ethanol or Methanol or IPA (50% v/v, 10 volumes per grams of ZLD-Ac form XII) (15 ml) was added drop-wise to a suspension of Zoledronic acid form XII (5.0 g) in a mixture of water (50% v/v)/Ethanol or Methanol or IPA (50% v/v, 10 volumes per grams of ZLD-Ac) (85 ml) at reflux temperature. The reaction mixture was heated at reflux temperature for additional 16 hours. Then the reaction mixture was cooled to room temperature. Further cooling was performed using an ice-bath. The precipitate was then filtered, washed and dried in a vacuum oven at 50° C. for 24 hours to give Zoledronate trisodium crystal form IX.

Workup

  1. additionwas added drop-wise
  2. temperatureat reflux temperature
  3. temperatureThe reaction mixture was heated
  4. temperatureat reflux temperature for additional 16 hours
  5. temperatureFurther cooling
  6. filtrationThe precipitate was then filtered
  7. washwashed
  8. customdried in a vacuum oven at 50° C. for 24 hours

Sources & evidence

ORD record
ord-687c501dff214e39a5a74763b2c17fc4
Source dataset
uspto-grants-2009_09
Patent number
US07582768B2

Reaction notes

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