反应 #1414906
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04081535
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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## were passed in at 0° C while cooling 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 was then heated (4-6 hours) After cooling the residue was filtered off washed with acetonitrile the total filtrate was evaporated under reduced pressure The crystalline residue was recrystallized from a little ethanol
来源 ID: ord-c3a0a818aa454d1ba9ae32cdd076a56b