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[目的]简化啶酰菌胺的合成方法,降低成本。[方法]以苯胺、4-氯苯肼、2-氯烟酰氯为原料,通过2步反应合成。关键的第1步反应优化条件:乙腈作溶剂,加料4-氯苯肼∶苯胺∶二氧化锰∶30%双氧水物质的量之比为1∶20∶0.1∶10。反应温度50℃,双氧水加料时间8 h,加料后反应时间5 h。[结果]啶酰菌胺总收率39%。[结论]该法避免使用钯催化剂及4-氯苯硼酸,具有路线短、原料价廉易得、氧化剂绿色无毒、反应条件温和等优点。
[Objective] To simplify the synthesis of boscalid and reduce the cost. [Method] Aniline, 4-chlorophenylhydrazine and 2-chloronicotinyl chloride were used as starting materials to synthesize by 2 steps. The key step 1 reaction optimization conditions: acetonitrile as a solvent, the amount of 4-chlorophenylhydrazine: aniline: manganese dioxide: 30% hydrogen peroxide content ratio of 1:20:0.1:10. Reaction temperature 50 ℃, hydrogen peroxide feed time 8 h, feed reaction time 5 h. [Result] The total yield of boscalid was 39%. [Conclusion] The method avoids the use of palladium catalyst and 4-chlorobenzene boronic acid, has the advantages of short route, cheap raw materials, non-toxic oxidant green, mild reaction conditions.