反应详情

Sodium (1.43 g) was added, with stirring under nitrogen, to dry ethanol (100 ml). After the sodium had dissolved a solution of N-cyano-N'-methyl-N"-(2-mercaptoethyl)guanidine (4.90 g) in dry ethanol (50 ml) was added and the mixture was stirred at room temperature for one hour. 5-Methyl-4-chloromethylimidazole hydrochloride (5.18 g) was added in batches over a period of one hour at room temperature. The mixture was then stirred at room temperature, for a further hour and heated at reflux temperature for 1/2 hour. After cooling the mixture was filtered and the filtrate was evaporated to a glassy solid (8.8 g). This crude product was chromatographed on silica gel with acetonitrile as eluant and the solid product obtained (3.60 g) was recrystallised from acetonitrile to give N-cyano-N'-methyl-"-[2-(5-methyl-4-imidazolylmethylthio)ethyl]guanidine, m.p.=140°-142° C.

1. additionwas added
2. stirringThe mixture was then stirred at room temperature, for a further hour
3. temperatureheated
4. temperatureat reflux temperature for 1/2 hour
5. temperatureAfter cooling the mixture
6. filtrationwas filtered
7. customthe filtrate was evaporated to a glassy solid (8.8 g)
8. customThis crude product was chromatographed on silica gel with acetonitrile as eluant
9. customthe solid product obtained (3.60 g)
10. customwas recrystallised from acetonitrile