Reaktion #645271

Reaktionsgleichung

N-{2-[N-(5-chloro(2-pyridyl))carbamoyl]-4-methylphenyl}(4-cyanophenyl)carboxamide

hydrogen chloride

N-methylethylenediamine

→

N-{2-[N-(5-chloro(2-pyridyl))carbamoyl]-4-methylphenyl}[4-(1-methyl(2-imidazolin-2-yl))phenyl]carboxamide

Lösungsmittel

methanol

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter 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
   Temperaturunder reflux condition for 2 hrs
5. 5
   SonstigeAfter the evaporation of solvent
6. 6
   Sonstigethe crude residue was purified by RP-HPLC

Vorschrift

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.

Quelle