微波法合成N,N′-二哌啶基硫脲及表征

Synthesis and characterization of N,N′-di-piperidi-1-thiourea under microwave irradiation

以硫脲的无水乙醇溶液和六氢吡啶为原料,在无催化剂的辐射作用下,探索制备N,N′-二哌啶基硫脲的工艺条件,并对其结构进行了表征.通过正交试验得出最佳的合成工艺条件:在微波仪温度-时间反应模式下,硫脲的无水乙醇溶液质量分数为1.56%,n(硫脲)∶n(六氢吡啶)=1∶2.2,搅拌速度500 r/min,55℃辐射反应9 min,收率可达65.78%.

Di-piperidin-l-thiourea was synthesized with ethanol solution of thiourea and hexahydropyridine in the absence of catalyst and microwave irradiation, and the structure of the product was characterized. The optimal experimental conditions were found through the orthogonal experiments： in the temperature-time response mode of microwave irradiation, ethanol solution of thiourea was 1.56%, n（thiourea）：n（hexahydropyridine）=1 ： 2.2, stirring speed was 500 r/min, reacted at 55 ℃ for 9 min. Under the optimal condition, the yield could reach 65.78%.