Risedronate → Risedronate sodium hemi-pentahydrate

HRID 217110

Reaction equation

HRID 217110 reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]([OH:17])([P:13]([OH:16])(=[O:15])[OH:14])[P:9]([OH:12])(=[O:11])[OH:10])[CH:2]=1.[OH-:18].[Na+:19]>O>[CH:5]1[CH:6]=[N:1][CH:2]=[C:3]([CH2:7][C:8]([P:9]([O-:11])([OH:12])=[O:10])([P:13]([OH:16])([OH:15])=[O:14])[OH:17])[CH:4]=1.[CH:5]1[CH:6]=[N:1][CH:2]=[C:3]([CH2:7][C:8]([P:9]([O-:11])([OH:12])=[O:10])([P:13]([OH:16])([OH:15])=[O:14])[OH:17])[CH:4]=1.[OH2:18].[OH2:10].[OH2:10].[OH2:10].[OH2:10].[Na+:19].[Na+:19]

Participants

4

Reactant 2

HCID 5245RisedronateHCID 14798Sodium Hydroxide

Product 1

HCID 11954322Risedronate sodium hemi-pentahydrateYield 194.1%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
25 °C

Procedure

To 60 ml of purified water, 10.0 g of 2-(3-pyridyl)-1-hydroxyethane-1,1-bisphosphonic acid (risedronic acid) and 1.41 g of sodium hydroxide were added and dissolved at an elevated temperature of 65° C. After the dissolution, the resulting solution was cooled to 25° C. over 3 hours for crystallization. The obtained crystals were filtered and vacuum dried to obtain 8.0 g of risedronate sodium hemipentahydrate (64.7% of theoretical yield). (LOD by TGA=13.2%)

Workup

  1. dissolutiondissolved at an elevated temperature of 65° C
  2. dissolutionAfter the dissolution
  3. filtrationThe obtained crystals were filtered
  4. customvacuum dried

Sources & evidence

ORD record
ord-9e6beb172792440a92180700437b9fb4
Source dataset
uspto-grants-2012_06
Patent number
US08193355B2

Linked notes

Loading…