反応 #48028

ord-cfd5e7ec58834f10b0e8e0e9c1b14b72

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the 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
    ろ過after filtration the solvent
  5. 5
    その他was evaporated in reduced pressure
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in the minimum amount of ethanol

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745465B2uspto-grants-2010_06