Methanol → HCID 86747508, compound

HRID 1198124Notes

Reaction equation

HRID 1198124 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-:23].[Na+].CO>O>[OH2:8].[OH2:23].[OH2:8].[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])([OH:21])[OH:22])[P:15](=[O:16])([OH:17])[OH:18]

Participants

5

Reactant 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 86747509HCID 86747509, compound

Product 1

HCID 86747508HCID 86747508, compoundYield 51%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

4-(2-Pyridyloxy)butylaminomethylenebisphosphonic acid hydrochloride (1.1 g) was dissolved in water (25 ml), to which was added an aqueous solution of sodium hydroxide (1N, 3 ml). To the mixture was added methanol to cause precipitation of a solid matter, which was collected by filtration and recrystallized from water-methanol to afford 4-(2-pyridyloxy)butylaminomethylenebisphosphonic acid trihydrate (0.6 g, 51%) as colorless crystals, m.p. 186° C. to 187° C.

Workup

  1. customprecipitation of a solid matter, which
  2. filtrationwas collected by filtration
  3. customrecrystallized from water-methanol

Sources & evidence

ORD record
ord-0e3963320b3a48e1aa79ec76347c690d
Source dataset
uspto-grants-1994_01
Patent number
US05280022

Reaction notes

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