反应详情

With 2 ml of acetonitrile were mixed 1 g of 2-{[2-(dimethylamino)methyl-4-thiazolyl]methylthio}ethylamine and 1.4 g of 1,1-bis(methylthio)-2-nitroethene, and the resulting mixture was subjected to reaction under reflux for 2 hours. After completion of the reaction, the solvent was removed by distillation under reduced pressure, and 5 ml of ethanol was added to the resulting residue, after which the insolubles were removed by filtration. The solvent was removed by distillation under reduced pressure, and the residue thus obtained was purified by a column chromatography (Wako Silica Gel C-200, eluent; chloroform:ethanol=20:1 by volume) to obtain 0.8 g (yield 53%) of oily 1-{2-[[2-(dimethylamino)methyl-4-thiazolyl]methylthio]ethylamino}-1-methylthio-2-nitroethene.

1. customthe resulting mixture was subjected to reaction
2. temperatureunder reflux for 2 hours
3. customAfter completion of the reaction
4. customthe solvent was removed by distillation under reduced pressure, and 5 ml of ethanol
5. additionwas added to the resulting residue
6. customafter which the insolubles were removed by filtration
7. customThe solvent was removed by distillation under reduced pressure
8. customthe residue thus obtained
9. customwas purified by a column chromatography (Wako Silica Gel C-200, eluent; chloroform:ethanol=20:1 by volume)