摘要
[目的]2-(4,5-二氢异唑-3-基)-3-甲基苯胺是一种重要农药中间体,简化合成方法,提高收率,以满足工业化生产需求。[方法]以3-硝基邻二甲苯为起始原料,经肟化反应得到2-甲基-6-硝基苯甲醛肟,然后与乙烯环合生成相应中间体,最后还原得到2-(4,5-二氢异恶唑)-3-甲基苯胺。目标化合物及中间体结构经1H NMR、MS确证。[结果]反应总收率63.6%,产品含量98.9%。[结论]该工艺收率高,操作简单,经济环保,条件温和,适合工业化生产。
[Aims] The purpose of this article is to explore and optimize the synthetic method of the 2-(4,5- dihydroisoxazol-3-yl)-3-methylaniline to meet the requirement of industrial production, which is a kind of important pesticide intermediate. [Methods] The 2-methyl-6-nitrobenzaldoxime can be obtained through substitution reaction using 3-nitro-o-xylene as starting material, followed by reacting with ethylene to get the corresponding intermediates, finally the 2- (4,5-dihydroisoxazol-3-yl)- 3- methylaniline was obtained through further reduction. The structures of the product and the intermediates were confirmed by 1H NMR and MS. [Results] The total yield was 63.6% and purity was as high as 98.9%. [Conclusions] The synthetic process has advantages of high yield, simple operation, economical and green process, which is suitable for industrial production.
出处
《农药》
CAS
CSCD
北大核心
2016年第11期790-792,813,共4页
Agrochemicals