反应详情

30.4 g (0.2 mole) of 2-phenoxyethylhydrazine were dissolved in 200 ml of anhydrous acetonitrile and 7.3 g of hydrogen chloride gas were passed in at 0° C. 32 g (0.2 mole) of N-chlorocarbonyl-isocyanide-dichloride were then added dropwise to the mixture at 15°-20° C, while cooling and stirring vigorously, and after completion of the addition, 30 g of potassium carbonate were also added. The batch was next stirred for 4 hours at room temperature, in the course of which the temperature in the reaction vessel at times rose to as much as 45° C, and was then heated under reflux until no further evolution of hydrogen chloride was detectable (4-6 hours). After cooling, the residue was filtered off and washed with acetonitrile, and the total filtrate was evaporated under reduced pressure. The crystalline residue was recrystallized from a little ethanol. 21 g (43.8% of theory) of 1-(2-phenoxyethyl)-5-chloro-3-hydroxy-1,2,4-triazole of melting point 166° C were obtained. ##STR100##

1. customwere passed in at 0° C
2. temperaturewhile cooling
3. additionwere also added
4. stirringThe batch was next stirred for 4 hours at room temperature, in the course of which the temperature in the reaction vessel at times
5. customrose to as much as 45° C
6. temperaturewas then heated
7. custom(4-6 hours)
8. temperatureAfter cooling
9. filtrationthe residue was filtered off
10. washwashed with acetonitrile
11. customthe total filtrate was evaporated under reduced pressure
12. customThe crystalline residue was recrystallized from a little ethanol