反应详情

A solution of methoxamine (7.0 g), prepared from the hydrochloride and potassium hydroxide in methanol (50 ml) and water (10 ml) was added to a solution of dimethylcyanodithioimidocarbonate (7.3 g) in methanol (40 ml) and stirred at room temperature for 60 hours. A solution of 4-methyl-5-[(2-aminoethyl)thiomethyl]imidazole (8.6 g) in methanol (30 ml) was added and the resulting solution was heated under reflux for 18 hours. Concentration followed by chromatographic purification on a column of silica gel with chloroform-methanol (10:1) as eluant and final recrystallisation from acetonitrile afforded the title compounds m.p. 155°-6°

1. temperaturethe resulting solution was heated
2. temperatureunder reflux for 18 hours
3. concentrationConcentration
4. customfollowed by chromatographic purification on a column of silica gel with chloroform-methanol (10:1) as eluant
5. customfinal recrystallisation from acetonitrile