反应详情

A solution of 1.43 g (0.0085 mole) of 2-(5-methyl-4-imidazolylmethylthio)ethylamine in dry acetonitrile (150 ml) was added dropwise, with stirring, to a solution of 1.43 g (0.0084 mole) of 1-methylthio-1-methyliminomethanesulphonate in dry acetonitrile (150) at 50°, giving an immediate white precipitation. After further warming at 70° for one hour, the mixture was stripped to dryness, dissolved in methanol and absorbed onto silica gel. Chromatography on a column of silica gel was performed with ethylacetate/methanol (20:1), and the crude product recrystallised from isopropanol to give the title compound, 0.46 g.m.p. 162.5°-163.5° as an almost colourless crystalline solid.

1. customgiving
2. customan immediate white precipitation
3. temperatureAfter further warming at 70° for one hour
4. dissolutiondissolved in methanol
5. customabsorbed onto silica gel
6. customthe crude product recrystallised from isopropanol