磺酰磺隆的合成

Synthesis of Sulfosulfuron

[目的]寻找具有工业化前景的除草剂磺酰磺隆的合成工艺。[方法]以2-氯咪唑[1,2-a]吡啶-3-磺酰胺为起始原料,先与乙硫醇钠反应合成2-乙硫基咪唑[1,2-a]吡啶-3-磺酰胺,再与双氧水反应合成2-乙磺酰基咪唑[1,2-a]吡啶-3-磺酰胺,最后与N-(4,6-二甲氧基嘧啶基-2-基)氨基甲酸苯酯反应合成磺酰磺隆。[结果]通过实验,确定了最佳路线,3步反应总收率68.1%,含量98.2%(HPLC)。[结论]该合成工艺具有步骤少、收率高、安全可靠的特点,可为工业化生产提供参考。

[Aims] The aim is to look for a preparation methold which is suitable for industrial production of the herbicide sulfosulfuron. [Methods] First, 2-chloroimidazo[1,2-a]pyridine-3-sulfonamide as starting mateiral was reacted with ethyl mercaptan sodium salt to synthesis 2-ethylthioimidazo[1,2-a]pyridine-3-sulfonamide. Then reacted with hydrogen peroxide solution to obtain 2-ethylsulfonylimidazo[1,2-a] pyridine-3-sulfonamide. Finally, sulfosulfuron was synthesized by the reaction of 2-ethylsulfonylimidazo[1,2-a]pyridine-3-sulfonamide with phenyl N-（4,6-dimethoxypyrimidin-2-yl） carbamate. [Results] The optimal method was determined by experiments. The total yield was 68.1%, and the purity of the product obtained is 98.2%（HPLC）. [Conclusions] The synthetic process has advantages of high yield, simple operation and safety, which is an important directive to industrialized production.