反应详情

2-Amino-1-methylimidazole hydrochloride (0.3 g) was dissolved in ethanol (4 ml), and sodium methoxide (28% methanol solution: 0.5 ml) and p-anisaldehyde (0.34 g) were added. The mixture was heated at reflux overnight. The solvent was evaporated. The residue was purified by silica gel column chromatography (eluent: methanol-chloroform=5:95), and the solvent in the desired fraction was evaporated. The precipitated pale yellow prisms were separated by filtration using hexane. The resulting crystals were dissolved in chloroform, and 4N hydrochloric acid--ethyl acetate (0.22 ml) was added. The solvent was evaporated, and the precipitated pale yellow was separated by filtration using diethyl ether to give the title compound (0.17 g, 26.9%).

1. temperatureThe mixture was heated
2. temperatureat reflux overnight
3. customThe solvent was evaporated
4. customThe residue was purified by silica gel column chromatography (eluent: methanol-chloroform=5:95)
5. customthe solvent in the desired fraction was evaporated
6. customThe precipitated pale yellow prisms were separated by filtration
7. dissolutionThe resulting crystals were dissolved in chloroform
8. addition4N hydrochloric acid--ethyl acetate (0.22 ml) was added
9. customThe solvent was evaporated
10. customthe precipitated pale yellow was separated by filtration