反应详情

An adaptation of the method described in WO 96/01826 was used. Imidazole-1-carbothioic acid (2-imino-2H-pyridin-1-yl)-amide (200 mg, 1.37 mmol) and 2-chloromethyl-1-methyl-4-phenyl-1H-imidazole 6 (300 mg, 1.46 mmol) were dissolved in 1-propanol (25 mL) and the mixture was heated to reflux for 2 hours. The solvent was removed under reduced pressure and the residue dissolved in dichloromethane. The solution was washed with water and the organic layer was dried over Na2SO4 and concentrated. The residue was purified by chromatography on silica gel to afford the title compound (273 mg, 62%) as a yellow solid. LC-MS: m/z=322.1 (MH+), tR=2.29 min, method B.

1. temperaturethe mixture was heated
2. temperatureto reflux for 2 hours
3. customThe solvent was removed under reduced pressure
4. dissolutionthe residue dissolved in dichloromethane
5. washThe solution was washed with water
6. dry with materialthe organic layer was dried over Na2SO4
7. concentrationconcentrated
8. customThe residue was purified by chromatography on silica gel