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除草剂甲基二磺隆的合成
Synthesis of Mesosulfuron-methyl
【摘要】 该文以对甲苯腈为原料,经氯磺化-氨解、氧化、还原、甲磺酰化、醇解反应制得关键中间体2-甲氧羰基-5-甲磺酰氨基甲基苯磺酰胺(Ⅵ),Ⅵ再与4,6-二甲氧基-2-(苯氧基羰基)氨基嘧啶反应得到目标产物甲基二磺隆(Ⅶ),6步反应总收率33.3%,产物及中间体经IR、1HNMR、MS确证结构。与文献合成工艺比较,该法具有原料易得,操作简便,收率高等优点。
【Abstract】 In this paper,the key intermediate of 2-methoxylcarbonyl-5-methylsulfonylaminomethyl-benzene sulfonamide(Ⅵ) was prepared starting from p-tolunitrile via chlorosulfonation-amination,oxidation,reduction,methylsulfonylation and alcoholysis.Subsequently,the target product of mesosulfuron-methyl(Ⅶ) was obtained from Ⅵ and 4,6-dimethoxy-2-(phenoxycarbonyl)aminopyrimidine.The total yield of the six steps was 33.3%.The structures of the target product and the intermediates were determined by IR,1HNMR and MS.Compared with the synthesis process in references,this synthetic route is characterized by cost-effectiveness,simple operation and high yield,holding out a brighter prospect for industrial application.
【Key words】 mesosulfuron-methyl; 2-methoxylcarbonyl-5-methylsulfonylaminomethylbenzene sulfonamide; 2-[(4,6-dimethoxypyrimidin-2-ylcarbamoyl)sulfamoyl]-α-(methanesulfoneamino)-p-toluic acid methyl ester; fine chemical intermediates;
- 【文献出处】 精细化工 ,Fine Chemicals , 编辑部邮箱 ,2013年03期
- 【分类号】TQ457.2
- 【被引频次】1
- 【下载频次】775