Sodium Hydroxide → HCID 131718313, compound

HRID 1198125Notes

Reaction equation

HRID 1198125 reaction equation
Cl.[N:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][CH2:9][CH2:10][CH2:11][CH2:12][NH:13][CH:14]([P:19](=[O:22])([OH:21])[OH:20])[P:15](=[O:18])([OH:17])[OH:16].[OH-].[Na+:24]>O>[OH2:8].[Na+:24].[Na+:24].[N:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][CH2:9][CH2:10][CH2:11][CH2:12][NH:13][CH:14]([P:19](=[O:20])([O-:21])[O-:22])[P:15](=[O:16])([OH:17])[OH:18]

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 86747509HCID 86747509, compound

Product 1

HCID 131718313HCID 131718313, compoundYield 62%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

4-(2-Pyridyloxy)butylaminomethylenebisphosphonic acid hydrochloride (2.0 g) was dissolved in water (50 ml), to which was added an aqueous solution of sodium hydroxide (1N, 15.9 ml). The reaction mixture was concentrated and then dissolved in water (50 ml). To the solution was added methanol to cause precipitation of a solid matter. The solid matter was collected by filtration and washed with methanol to give 4-(2-pyridyloxy)butylaminomethylenebisphosphonic acid disodium salt monohydrate (1.3 g, 62%) as colorless crystals, m.p.>300° C.

Workup

  1. concentrationThe reaction mixture was concentrated
  2. dissolutiondissolved in water (50 ml)
  3. additionTo the solution was added methanol
  4. customprecipitation of a solid matter
  5. filtrationThe solid matter was collected by filtration
  6. washwashed with methanol

Sources & evidence

ORD record
ord-92ab83a612ce48029121d5fe2eddc30e
Source dataset
uspto-grants-1994_01
Patent number
US05280022

Reaction notes

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