氟噻虫砜的合成工艺

Synthetic Process of Fluensulfone

[目的]降低氟噻虫砜的合成成本,提高合成效率。[方法]以二硫化碳为原料,制得二硫代氨基甲酸铵,经环化、取代、氯化、氧化得氟噻虫砜。[结果]化合物结构经1H NMR确认,对环化反应的工艺条件进行优化,最佳反应条件:n(二硫代氨基甲酸铵)∶n(氯乙醛)∶n(浓盐酸)为1∶1∶1.5,2-巯基噻唑收率为88.3%,目标产物总收率为51.5%。[结论]该合成工艺步骤短,所用原料易得,产品收率高,安全环保、可实现工业化生产、符合绿色经济的要求。

[Aims] Reduce the synthetic cost of fluensulfone and improve the synthesis efficiency. [Methods] Fluensulfone was synthesized by several steps such as cyclization, substitution, chlorination and oxidation with the raw material ammonium dithiocarbamate which synthesized by carbon disulfide. [Results] The structures of the compounds were confirmed by 1H NMR, and the reaction condition of the cyclization was optimized, n(ammonium dithiocarbamate)∶n(chloroacetaldehyde)∶n(concentrated hydrochloric acid) was 1∶1∶1.5, the yield of 2-mercaptothiazole was 88.3%, and the total yield of the target product was 51.5%. [Conclusions] This route of synthesizing fluensulfone could reduce the step and obtain a good yield with the raw material which easy to purchase, meanwhile, it would be a green way to realize the industrial production.