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

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.

1. customAfter the evaporated the solvent
2. dissolutionthe residue was dissolved in anhydrous methanol (5 ml)
3. stirringThe mixture was stirred
4. temperatureunder reflux condition for 2 hrs
5. customAfter the evaporation of solvent
6. customthe crude residue was purified by RP-HPLC

ORDレコード

ord-7769d72acc204e3c94f7a4faf46f2404

出典データセット

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07727982B2