Tributylamine → Clodronate

HRID 1181911Notes

Reaction equation

HRID 1181911 reaction equation
[Na+].[Na+].[Cl:3][C:4]([Cl:13])([P:9](=[O:12])([O-:11])[O-:10])[P:5](=[O:8])([OH:7])[OH:6].C(N(CCCC)CCCC)CCC>>[Cl:13][C:4]([Cl:3])([P:5](=[O:6])([OH:8])[OH:7])[P:9](=[O:10])([OH:11])[OH:12]

Participants

3

Reactant 2

HCID 7622TributylamineHCID 73554303Dichloromethylenediphosphonic acid

Product 1

HCID 25419Clodronate

Procedure

An aqueous solution of dichloromethylenediphosphonic acid disodium salt (1.0 g, 3.46 mmol) was loaded on a column of DOWEX 50WX8-100 ion-exchange resin and eluted with water. Tributylamine (1.65 mL, 6.92 mmol) was added and the mixture was shaken vigorously. The resulting solution was concentrated to dryness and coevaporated with anhydrous DMF three times. The residue was dried under vacuum overnight.

Workup

  1. washeluted with water
  2. concentrationThe resulting solution was concentrated to dryness
  3. customThe residue was dried under vacuum overnight

Sources & evidence

ORD record
ord-b00d9609df3e4f67bd077843cb0cb932
Source dataset
uspto-grants-2007_10
Patent number
US07285658B2

Reaction notes

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