Risedronate → Risedronate Sodium

HRID 2265923Notes

Reaction equation

HRID 2265923 reaction equation
[CH:1]1[CH:6]=[N:5][CH:4]=[C:3]([CH2:7][C:8]([P:14]([OH:17])([OH:16])=[O:15])([P:10]([OH:13])([OH:12])=[O:11])[OH:9])[CH:2]=1.[OH-].[Na+:19]>O>[CH:1]1[CH:6]=[N:5][CH:4]=[C:3]([CH2:7][C:8]([P:10]([O-:12])([OH:13])=[O:11])([P:14]([OH:17])([OH:16])=[O:15])[OH:9])[CH:2]=1.[Na+:19]

Participants

4

Reactant 2

HCID 5245RisedronateHCID 14798Sodium Hydroxide

Product 1

HCID 4194514Risedronate Sodium

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

21.0 g of risedronic acid and 700 ml of deionized water are charged into a 1-liter reactor, equipped with mechanical stirrer and thermometer. The suspension, under stirring, is added with 148.4 ml of NaOH 0.5N thus obtaining complete dissolution of the suspended solid. The pH of the solution is 4.67. The solution is kept under stirring for 10′ and filtered on a paper filter and put into Lioguard chambers. The chambers are introduced into a lyophilizer which is set according to the following parameters: a) freezing-phase: temperature −40° C., freezing time 3 hours; b) lyophilization phase: time 89 hours, internal temperature 30° C., residual vacuum 400÷450 μHg. At the end of the process, the white and soft product is discharged from the chambers. 20.9 g of lyophilized amorphous sodium risedronate are thus obtained (yields 92.3%).

Workup

  1. customequipped with mechanical stirrer
  2. customthus obtaining complete
  3. dissolutiondissolution of the suspended solid
  4. stirringunder stirring for 10′ and
  5. filtrationfiltered on a paper
  6. filtrationfilter
  7. additionThe chambers are introduced into a lyophilizer which
  8. customtemperature −40° C.
  9. customtime 3 hours
  10. customtime 89 hours, internal temperature 30° C., residual vacuum 400÷450 μHg

Sources & evidence

ORD record
ord-40bbd9a535d34c299c17ecc0163d1fd6
Source dataset
uspto-grants-2010_12
Patent number
US07858634B2

Reaction notes

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