반응 #601905

반응 방정식

N-{6-[N-(5-bromo(2-pyridyl))carbamoyl]-2,3,4-trimethoxyphenyl}(4-cyanophenyl)carboxamide

hydrogen chloride

N-methylethylenediamine

→

N-{6-[N-(5-bromo(2-pyridyl))carbamoyl]-2,3,4-trimethoxyphenyl}[4-(1-methyl(2-imidazolin-2-yl))phenyl]carboxamide

수율 32.0%

용매

methanol

ethyl acetate

반응 조건

후처리

1. 1
   기타After 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
   온도under reflux condition for 2 hrs
5. 5
   기타After the evaporation of solvent
6. 6
   기타the crude residue was purified by RP-HPLC

실험 절차

To a solution of the compound of N-{6-[N-(5-bromo(2-pyridyl))carbamoyl]-2,3,4-trimethoxyphenyl}(4-cyanophenyl)carboxamide (680 mg, 1.33 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 (0.586 ml, 6.65 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-{6-[N-(5-bromo(2-pyridyl))carbamoyl]-2,3,4-trimethoxyphenyl}[4-(1-methyl(2-imidazolin-2-yl))phenyl]carboxamide as a white powder (240 mg, 32%). MS found for C26H26BrN5O5 M+=568, (M+2)+=570.

출처