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以2-氯-5-氯甲基吡啶(CCMP)、无水乙二胺和硝基胍为原料,运用串联反应方法合成了吡虫啉[化学名:1-(6-氯-3-吡啶甲基)-N-硝基-2-咪唑啉亚胺]。该方法反应中间体无需纯化处理,操作简单,同时解决了活性中间体进一步进行副反应的难题。通过单因素实验,探讨了pH、反应溶剂、温度以及时间等因素对产物收率的影响,得到的优化工艺条件为:以乙腈为溶剂,nCCMP∶n无水乙二胺∶n硝基胍=1∶5∶1,于30℃反应120min,产率可达96.35%。其结构经1H NMR、13C NMR、IR表征。
The imidacloprid [Chemical Name: 1- (6-Chloro-3-picolylmethyl) imidazole was synthesized from 2-chloro-5-chloromethylpyridine (CCMP), anhydrous ethylenediamine and nitroguanidine by a tandem reaction ) -N-nitro-2-imidazolidinimine]. The method does not require the intermediates to be purified, and the operation is simple. Meanwhile, the problem of further side reactions of the active intermediates is solved. Through single factor experiments, the effects of pH, reaction solvent, temperature and time on the yield of the product were discussed. The optimum technological conditions were as follows: acetonitrile as solvent, nCCMP:n anhydrous ethylenediamine: n nitroguanidine = 1: 5: 1, at 30 ℃ for 120min, the yield can reach 96.35%. Its structure was characterized by 1H NMR, 13C NMR, IR.