反应详情

To a solution of the above isothiourea (5.0 g, 9.133 mmol) in dry pyridine (70 ml) was added 3-(1H-imidazol-4-yl)propyl amine (1.26 g, 10.05 mmol) and the resulting mixture was stirred at reflux temperature for 10 h followed by stirring at room temperature for 48 h. The solvent was evaporated in vacuo and the residue was purified by column chromatography on silica gel (600 ml) using a mixture of dichloromethane/methanol/triethylamine 9:0.5:0.5 as eluent affording 3.31 g (58%) of the title compound as an amorphous solid.

1. temperatureat reflux temperature for 10 h
2. stirringby stirring at room temperature for 48 h
3. customThe solvent was evaporated in vacuo
4. customthe residue was purified by column chromatography on silica gel (600 ml)
5. additiona mixture of dichloromethane/methanol/triethylamine 9:0.5:0.5 as eluent