章瑛,王宏亮,吴建一.化学通报,2014,77(9):919-921. |
基于串联反应的吡虫啉新合成工艺研究 |
New Study on Synthesis Technology of Imidacloprid via Cascade Reaction |
投稿时间:2014-01-14 修订日期:2014-01-30 |
DOI: |
中文关键词: 2-氯-5-氯甲基吡啶 串联反应 吡虫啉 合成 |
英文关键词:2-chloro-5-chloromethyl pyridine cascade reaction imidacloprid synthesize |
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中文摘要: |
以2-氯-5-氯甲基吡啶、无水乙二胺和硝基胍为原料,运用串联反应的新方法合成了吡虫啉(化学名:1-(6-氯-3-吡啶甲基)-N-硝基-2-咪唑啉亚胺)。该方法无需处理中间体,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值、反应溶剂、温度以及时间等因素对产物收率的影响,得到的最佳工艺条件为:以乙腈为溶剂,n(CCMP):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。 |
英文摘要: |
Imidacloprid was synthesized using a new method by the cascade reaction of 2-chloro-5-chloromethyl pyridine, 1,2-ethanediamine and nitroguanidine. This method was very easy without treatment with intermediate, while resolving the existence of side-reation. The effects of pH, solvents, temperature and time on the yield of imidacloprid were investigated. The optimum reaction conditions at 30℃ for 120min were as follows: n(CCMP):n(1,2-ethanediamine):n(nitroguanidine) was 1:5:1 in acetonitrile. The yield was 96.35% under the optimum conditions. The structure was characterized by 1H ,13C and IR. |
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