啶酰菌胺的合成  

Studies on the Synthesis of Boscalid

作　　者：程传杰[1] 曹星星[1] 白雄雄[1] 夏红英[1] 黄庆华[1] 胡仲禹[1] 

机构地区：[1]江西科技师范大学化学化工学院,南昌330013

出　　处：《农药》2016年第2期96-98,110,共4页Agrochemicals

基　　金：国家自然科学基金(21264008;21564004);江西省自然科学基金项目(2009GZH0035)

摘　　要：[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。[Aims] This paper aims to simplify the synthetic method for bactericide boscalid to reduce cost. [Methods]Boscalid was successfully synthesized via two steps, using aniline, 4-chlorophenyl hydrazine and 2-chloronicotinoyl chloride as the main reactants. The optimized conditions for the key coupling reaction were： Me CN as the solvent;molar ratio of feedstock was 4-chlorophenyl hydrazine ∶aniline ∶manganese dioxide ∶30% H2O2=1 ∶20 ∶0.1 ∶10; reaction temperature was 50 ℃; time for the addition of hydrogen peroxide was 8 h, followed by further stirring for 5 h.[Results] Total yield of boscalid was 39% under optimized conditions. [Conclusions] The method has some advantages of avoiding using noble-metal palladium catalyst and expensive 4-chlorophenyl boronic acid, less reaction steps, cheap reagents, green oxidant, and mild reaction conditions.

关 键 词：啶酰菌胺 杀菌剂 偶联反应 

分 类 号：TQ455[化学工程—农药化工]