تفاعل #48028

ord-cfd5e7ec58834f10b0e8e0e9c1b14b72

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe 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
    ترشيحafter filtration the solvent
  5. 5
    أخرىwas evaporated in reduced pressure
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in the minimum amount of ethanol

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745465B2uspto-grants-2010_06