HCID 15227696, compound → HCID 131718817, compound

HRID 1492890Notes

Reaction equation

HRID 1492890 reaction equation
[N:1]1[CH:6]=[CH:5][C:4]([S:7][CH2:8][CH2:9][CH2:10][NH:11][CH:12]([P:21](=[O:28])([O:25]CC)[O:22]CC)[P:13](=[O:20])([O:17]CC)[O:14]CC)=[CH:3][CH:2]=1>Cl>[OH2:14].[N:1]1[CH:6]=[CH:5][C:4]([S:7][CH2:8][CH2:9][CH2:10][NH:11][CH:12]([P:21](=[O:22])([OH:25])[OH:28])[P:13](=[O:14])([OH:17])[OH:20])=[CH:3][CH:2]=1.[N:1]1[CH:6]=[CH:5][C:4]([S:7][CH2:8][CH2:9][CH2:10][NH:11][CH:12]([P:21](=[O:22])([OH:25])[OH:28])[P:13](=[O:14])([OH:17])[OH:20])=[CH:3][CH:2]=1

Participants

3

Reactant 1

HCID 15227696HCID 15227696, compound

Product 1

HCID 131718817HCID 131718817, compoundYield 112.8%

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

A mixture of tetraethyl 3-(4-pyridylthio)propylaminomethylenebisphosphonate (7.4 g) and concentrated hydrochloric acid (50 ml) was heated under reflux for 2 hours, and then concentrated under reduced pressure. The residual crystals were collected by filtration to obtain 3-(4-pyridylthio)propylaminomethylenebisphosphonic acid hemihydrate (4.3 g, 77%), and recrystallized from water.

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. concentrationconcentrated under reduced pressure
  4. filtrationThe residual crystals were collected by filtration

Sources & evidence

ORD record
ord-15837df2f0fc4f24b3ae420d4e3ac96a
Source dataset
uspto-grants-1994_12
Patent number
US05376647

Reaction notes

Loading…