摘要
研究了以邻甲酸甲酯苄基磺酰氯、2-氨基-4,6-二甲氧基嘧啶和氰酸钠为原料,乙腈为溶剂,在吡啶催化下合成除草剂苄嘧磺隆的新方法。考察了溶剂种类、催化剂用量、氰酸钠用量、反应时间、反应温度等因素对反应的影响。结果表明:邻甲氧羰基苄基磺酰氯、2-氨基-4,6-二甲氧基嘧啶、吡啶和氰酸钠摩尔比为1∶1∶1∶1.2,乙腈为溶剂,在40°C下搅拌反应3 h,产品收率67.8%,纯度97.0%(HPLC)。该方法避免了剧毒光气,简化了工艺路线,是一个对环境友好的磺酰脲除草剂的合成方法。
Herbicide bensulfuron-methyl was prepared by reaction of methyl 2-(chlorosulfonylmethyl) benzoate with sodium cyanate and 2-amino-4, 6-dimethoxypyrimidine in the presence of pyridine as a catalyst in acetonitrile. The effects of kind of solvent, amounts of catalyst and sodium cyanate, reaction time and reaction temperature were studied. The optimum conditions are as follows: molar ratio of methyl 2-(chlorosulfonylmethyl) benzoate : g-amino-4,6-dimethoxypyrimidine : pyridine : sodium cyanate=1 : 1 : 1 : 1.2, acetonitrile as a solvent, reaction time 3 h, reaction temperature 40℃. The yield and purity of product is 67.8%, and 97% (HPLC), respectively. The method can secure from using phosgene and the process is simple. It is a green chemical method for preparation of sulfonylurea herbicides.
出处
《化学世界》
CAS
CSCD
北大核心
2008年第11期685-687,共3页
Chemical World
关键词
除草剂
苄嘧磺隆
合成
氰酸钠
herbicide
bensul
uron-methyl
synthesis
sodium cyanate