Reaktion #48028

ord-cfd5e7ec58834f10b0e8e0e9c1b14b72

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe mixture was evaporated to dryness
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in 300 ml of methanol
  3. 3
    workup.ADDITIONtreated with charcoal
  4. 4
    Filtrationafter filtration the solvent
  5. 5
    Sonstigewas evaporated in reduced pressure
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in the minimum amount of ethanol

Vorschrift

17.5 g (0.05 mole) of N-[2-hydroxy-3-(1-piperidinyl)propoxy]-3-pyridinecarboximidamide dihydrochloride was dissolved in 50 ml of thionyl chloride, boiled for one hour, then the mixture was evaporated to dryness. The residue was dissolved in 300 ml of methanol, treated with charcoal and after filtration the solvent was evaporated in reduced pressure. The residue was dissolved in the minimum amount of ethanol and refrigerated to yield crystalline N-[2-chloro-3-(1-piperidinyl)propoxy]-3-pyridine-carboximidamide dihydrochloride as intermediate compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745465B2uspto-grants-2010_06