2_6_二乙基_4_甲基苯基丙二酰胺的合成_陈立鹏.pdf

第53卷第8期 农 药 Vol. 53, No. 8 2014年8月 Agrochemicals Aug. 2014 陈立鹏, 廖道华, 高倩, 等. 2,6-二乙基-4-甲基苯基丙二酰胺的合成[J]. 农药, 2014, 53(8): 558-560. 2,6-二乙基-4-甲基苯基丙二酰胺的合成 陈立鹏，廖道华，高 倩，李爱军，郭 栋，岳 航，杨 帆 (华东理工大学 药学院， 上海 200237) 摘要：[目的]旨在探索并优化出一条适合工业化生产2,6-二乙基-4-甲基苯基丙二酰胺的工艺路线。 [方法] 2,6- 二乙基-4-甲基苯胺经过Sandmeyer反应，得到2,6-二乙基-4-甲基溴苯，然后与丙二腈在氯化钯催化下偶合，得 到2,6-二乙基-4-甲基苯基丙二腈，最后将其水解得到目标产物2,6-二乙基-4-甲基苯基丙二酰胺。 [结果]反应 总收率为71.8%，产物与中间体经1H NMR、MS等进行了表征。 [结论]该路线收率较高，原料易得，实验步骤较少， 适合工业生产。 关键词：唑啉草酯；中间体；除草剂；合成 中图分类号：TQ460.3 文献标志码：A 文章编号：1006-0413(2014)08-0558-03 The Synthesis of 2-(2,6-diethyl-4-methylphenyl)malonamide CHEN Li-peng, LIAO Dao-hua, GAO Qian, LI Ai-jun, GUO Dong, YUE Hang, YANG Fan (Pharmacy school, East China University of Science and Technology, Shanghai 200237, China) Abstract: [Aims] This article aims to explore and optimize a reasonable route of 2-(2,6-diethyl-4-methylphenyl) malonamide on industrial scale. [Methods] 2,6-diethyl-4-methyl-bromobenzene was prepared from 2,6-diethyl-4-methyl- aniline by the Sandmeyer reaction, then coupled with malononitrile under palladium catalysis to give the 2,6-diethyl-4- methyl-phenyl-malononitrile, which was hydrolyzed to get the target product. [Results] The total yield of the process was 71.8%, and the important intermediate and products were characterized by MS and 1H NMR. [Conclusions] The proposed synthetic route has many advantages, including high yield, easily available raw materials, few synthetic steps and it can be suitable for industrial production