Hydrochloric Acid → HCID 86748345, compound

HRID 1492889Notes

Reaction equation

HRID 1492889 reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7][CH2:8][CH2:9][CH2:10][CH2:11][NH:12][CH:13]([P:22](=[O:29])([O:26]CC)[O:23]CC)[P:14](=[O:21])([O:18]CC)[O:15]CC.[ClH:30]>>[ClH:30].[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7][CH2:8][CH2:9][CH2:10][CH2:11][NH:12][CH:13]([P:22](=[O:23])([OH:26])[OH:29])[P:14](=[O:15])([OH:18])[OH:21]

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 15230149HCID 15230149, compound

Product 1

HCID 86748345HCID 86748345, compoundYield 70%

Procedure

A solution of tetraethyl 4-(2-pyridylthio)butylaminomethylenebisphosphonate (2.50 g) in hydrochloric acid (40 ml) was stirred for 3 hours under reflux. The reaction mixture was concentrated under reduced pressure. Acetone was added to the residue and the separated white precipitate was collected by filtration and recrystallized from water-methanol to obtain 4-(2-pyridylthio)butylaminomethylenebisphosphonic acid hydrochloride (1.46 g, 70%) as a white powder.

Workup

  1. temperatureunder reflux
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionAcetone was added to the residue
  4. filtrationthe separated white precipitate was collected by filtration
  5. customrecrystallized from water-methanol

Sources & evidence

ORD record
ord-19a77bf180384faa8c83c0663b044236
Source dataset
uspto-grants-1994_12
Patent number
US05376647

Reaction notes

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