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.
出处
《农药》
CAS
CSCD
北大核心
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)
关键词
啶酰菌胺
杀菌剂
偶联反应
boscalid
bactericide
coupling reaction
