反应详情

To a solution of sodium metal (1.01 g) in ethanol (120 ml) were added cyanamide (18.5 g) and N-cyano-S-methyl-N'-[2-(5-methylimidazol-4-ylmethylthio)ethyl]isothiourea (10.76 g). The resulting mixture was heated under reflux for 1.5 hrs. After concentration under a reduced pressure, the residue was added to cold water (50 ml) and acidified (pH 4.5) with 10% HCl and cooled for 1 hr. in an ice bath. The precipitate was filtered, washed with water and dried. The resulting crude product (7.43 g) was recrystallized from C2H5OH-H2O (1:1) to give N,N'-dicyano-N"-[2-(5-methylimidazol-4-ylmethylthio)ethyl]guanidine (5.17 g).

1. temperatureThe resulting mixture was heated
2. temperatureunder reflux for 1.5 hrs
3. concentrationAfter concentration under a reduced pressure
4. additionthe residue was added to cold water (50 ml)
5. temperaturecooled for 1 hr
6. filtrationThe precipitate was filtered
7. washwashed with water
8. customdried
9. customThe resulting crude product (7.43 g) was recrystallized from C2H5OH-H2O (1:1)