Sodium Methoxide → HCID 23297363, compound

HRID 1198122Notes

Reaction equation

HRID 1198122 reaction equation
[O:1]([CH2:8][CH2:9][CH2:10][CH2:11][NH:12][CH:13]([P:18](=[O:21])([OH:20])[OH:19])[P:14](=[O:17])([OH:16])[OH:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[O-].[Na+:24]>CO>[Na+:24].[Na+:24].[O:1]([CH2:8][CH2:9][CH2:10][CH2:11][NH:12][CH:13]([P:18](=[O:19])([O-:20])[O-:21])[P:14](=[O:15])([OH:16])[OH:17])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 10942334Sodium MethoxideHCID 23184155HCID 23184155, compound

Product 1

HCID 23297363HCID 23297363, compoundYield 91.8%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

4-Phenoxybutylaminomethylenebisphosphonic acid (0.54 g) was suspended in methanol (20 ml), to which was added a methanol solution of sodium methoxide (28%, 0.782 g), and the mixture was stirred for 3 hours at room temperature. The reaction mixture was concentrated under reduced pressure. The concentrate was treated with acetone to give a solid matter, which was recrystallized from water-methanol to give 4-phenoxybutylaminomethylenebisphosphonic acid disodium salt 1.5 hydrate (0.56 g, 85%), m.p.>300° C.

Workup

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionThe concentrate was treated with acetone
  3. customto give a solid matter, which
  4. customwas recrystallized from water-methanol

Sources & evidence

ORD record
ord-13d572317bdf47b898df90719268834e
Source dataset
uspto-grants-1994_01
Patent number
US05280022

Reaction notes

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