Réaction #40433

ord-fc958fa311974f6596f2ee991a7694ea

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreAfter the evaporated the solvent
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in anhydrous methanol (5 ml)
  3. 3
    workup.STIRRINGThe mixture was stirred
  4. 4
    Températureunder reflux condition for 2 hrs
  5. 5
    AutreAfter the evaporation of solvent
  6. 6
    Autrethe crude residue was purified by RP-HPLC

Mode opératoire

To a lotion of the compound of N-{2-[N-(5-chloro(2-pyridyl))carbamoyl]-4-methylphenyl}(4-cyanophenyl)carboxamide (830 mg, 2.1 mmol) in anhydrous methanol (5 ml) and ethyl acetate (10 ml) was saturated with hydrogen chloride gas at 0° C. The mixture was stirred at r.t. overnight. After the evaporated the solvent, the residue was dissolved in anhydrous methanol (5 ml) and N-methylethylenediamine (0.926 ml, 10.5 mmol) was added. The mixture was stirred under reflux condition for 2 hrs. After the evaporation of solvent, the crude residue was purified by RP-HPLC to give N-{2-[N-(5-chloro(2-pyridyl))carbamoyl]-4-methylphenyl}[4-(1-methyl(2-imidazolin-2-yl))phenyl]carboxamide as a white powder. MS found for C24H22ClN5O2 M+=448, (M+2)+=450.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07727981B2uspto-grants-2010_06