反应详情

17 g (0.2 mole) of 2-cyanoethylhydrazine were dissolved in 100 ml of acetonitrile and 7.3 g of hydrogen chloride gas were passed in at -10° C. Thereafter, 32 g of N-chlorocarbonylisocyanide dichloride were added dropwise at 0° C., whilst cooling and stirring well, and after completion of this addition, 30 g of potassium carbonate were added. This mixture was first stirred for 2 hours at room temperature and was then heated under reflux until no further evolution of hydrogen chloride was detectable (5 to 6 hours). After cooling, the mixture was filtered, the residue was washed with acetonitrile and the entire filtrate was concentrated by evaporation in vacuo. The oil which remained was taken up in a little ethanol and cooled to -10° to -15° C. The colorless crystals which had precipitated were filtered off and dried. 20 g of 1-(2-cyanoethyl)-5-chloro-3-hydroxy-1,2,4-triazole of melting point 149°-150° C. were obtained. ##STR23##

1. customwere passed in at -10° C
2. temperaturewhilst cooling
3. additionwere added
4. stirringThis mixture was first stirred for 2 hours at room temperature
5. temperaturewas then heated
6. custom(5 to 6 hours)
7. temperatureAfter cooling
8. filtrationthe mixture was filtered
9. washthe residue was washed with acetonitrile
10. concentrationthe entire filtrate was concentrated by evaporation in vacuo
11. temperaturecooled to -10° to -15° C
12. customThe colorless crystals which had precipitated
13. filtrationwere filtered off
14. customdried