【摘要】 [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。更多还原

【Abstract】 [Aims] This article aims to obtain a reasonable route of metazosulfuron on industrial scale. [Methods] Ethyl [[3-chloro-1-methyl-4-(5-methyl-5,6-dihydro-1,4,2-dioxazin-3-yl)-1H-pyrazol-5-yl]sulfonyl]carbamate was obtained from 3-chloro-4-methoxycarbonyl-5-sulfamoyl-1-methylpyrazole via condensation, hydrolysis, chloroformylation, condensation, and cyclization. Then it was reacted with 2-amino-4,6-dimethoxy pyrimidine to get metazosulfuron. [Results] The total yield was 47.9%, and the purity of metazosulfuron was 97.7%(HPLC). The products and intermediates were determined by 1H NMR and MS and so on. [Conclusions] The route has advantages of easily available raw material, high yield, simple operations and mild conditions, which lays the foundation for industrial production.更多还原