反应详情

To a solution of 2-chloro-1-(4-methylpyridin-2-yl)propan-1-one (0.4 g) in ethanol (5 ml) was added 2-imino-4-thiobiuret (257 mg). The mixture was refluxed for 2 hours, and the solvent was evaporated under reduced pressure. To the residue were added ethyl acetate and a saturated aqueous sodium hydrogencarbonate solution. The ethyl acetate layer was separated, washed with brine, dried over sodium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 25 g, dichloromethane:methanol:triethylamine=80:10:1) to give 2-guanidino-5-methyl-4-(4-methylpyridin-2-yl)thiazole (402 mg).

1. temperatureThe mixture was refluxed for 2 hours
2. customthe solvent was evaporated under reduced pressure
3. additionTo the residue were added ethyl acetate
4. customThe ethyl acetate layer was separated
5. washwashed with brine
6. dry with materialdried over sodium sulfate
7. customevaporated under reduced pressure
8. customThe residue was purified by column chromatography (silica gel 25 g, dichloromethane:methanol:triethylamine=80:10:1)