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[目的]旨在找出一条适合工业化生产双醚氯吡嘧磺隆的工艺路线。[方法]以3-氯-1-甲基吡唑-4-甲酸甲酯-5-磺酰胺为原料,通过缩合、水解、酰氯化、缩合、环化得到3-氯-1-甲基吡唑-4-(5-甲基-5,6-二氢-1,4,2-二嗪-3-基)-5-磺酰基氨基甲酸乙酯,最后与2-氨基-4,6-二甲氧基嘧啶反应得到双醚氯吡嘧磺隆。[结果]该合成路线共6步,产物及中间体经MS、1H NMR等进行表征,反应总收率为47.9%,双醚氯吡嘧磺隆含量为97.7%(HPLC)。[结论]该方法具有原料易得、反应条件温和、操作简单易行、收率较高等特点,为工业化生产奠定了基础。
[Objective] The aim was to find out a technological route suitable for the industrial production of bis-chlorosulfuron-methyl. [Method] Starting from 3-chloro-1-methylpyrazole-4-carboxylic acid methyl ester 5-sulfonamide, condensation, hydrolysis, acid chlorination, condensation and cyclization gave 3-chloro- Oxazol-4- (5-methyl-5,6-dihydro-1,4,2-diazin-3-yl) -5-sulfonylcarbamate and finally 2-amino-4,6- Dimethoxypyrimidine reaction to give bis-chloro-pyrazosulfuron-methyl. [Result] The synthetic route was 6 steps. The products and intermediates were characterized by MS, 1H NMR and so on. The total yield of the reaction was 47.9%, and the content of TCTD was 97.7% (HPLC). [Conclusion] The method has the advantages of easy-to-obtain raw materials, mild reaction conditions, simple and easy operation and high yield, which laid the foundation for industrialized production.