环氧虫啶的合成工艺研究
发布时间：2018-07-20 15:29
【摘要】：环氧虫啶是华东理工大学发现的具有自主知识产权的、结构新颖的新烟碱类杀虫剂,对吡虫啉的抗性害虫具有显著活性,而且对鳞翅目害虫也具有较好的防治效果。目前环氧虫啶正在产业开发中,确定并优化工艺路线、降低生产成本是环氧虫啶实现产业化并最终走向市场的关键。 本论文的目的是对环氧虫啶的合成路线进行分析,确定其工艺路线并进行优化,达到适合工业化生产的要求。在环氧虫啶专利合成路线的基础上,根据其结构特点,设计三条路线并进行评估,确定了一条可行的工艺路线：以偏二氯乙烯为起始原料,经过硝化、环合、缩合得到硝基亚甲基中间体。此中间体与2,5-二甲氧基四氢呋喃经水解得到的丁二醛反应、再环合得到环氧虫啶。 本论文对确定的路线中每步反应进行合成条件及后处理的优化,讨论了各种因素对反应的影响,从中得到了合成环氧虫啶的较佳工艺条件。成本由原来的169万元/吨下降到约87万元／吨。各步反应条件温和,操作简单,避免了甲硫醇的排放及过量乙二胺的使用,是一条更加绿色环保、具有工业化开发前景的路线。
[Abstract]:Epoxidin is a new nicotinic insecticide with its own intellectual property rights and novel structure, which has remarkable activity against imidacloprid pests and has good control effect on Lepidoptera pests. At present, epoxidin is in the process of industrial development. To determine and optimize the technological route and reduce the production cost is the key to realize the industrialization of epoxidin and finally to enter the market. The purpose of this paper is to analyze the synthetic route of epoxidin, determine its technological process and optimize it to meet the requirements of industrial production. Based on the synthetic route of epoxide patent, according to its structural characteristics, three routes were designed and evaluated, and a feasible technological route was determined: using vinylidene chloride as the starting material, nitration, cyclization, nitration and cyclization. The intermediate of nitromethylene was obtained by condensation. The intermediate reacts with 2-dimethoxytetrahydrofuran to hydrolyze succinaldehyde and cyclization to obtain epoxide. In this paper, the synthesis conditions and post-treatment of each reaction in the determined route were optimized, and the effects of various factors on the reaction were discussed, from which the better technological conditions for the synthesis of cycloprozidine were obtained. The cost dropped from 1.69 million yuan / ton to about 870000 yuan / ton. The reaction conditions are mild, the operation is simple, the emission of methionol and the use of excessive ethylenediamine are avoided, which is a more green and environmentally friendly route with the prospect of industrial development.
【学位授予单位】：华东理工大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：TQ453.2
本文编号：2133972
[Abstract]:Epoxidin is a new nicotinic insecticide with its own intellectual property rights and novel structure, which has remarkable activity against imidacloprid pests and has good control effect on Lepidoptera pests. At present, epoxidin is in the process of industrial development. To determine and optimize the technological route and reduce the production cost is the key to realize the industrialization of epoxidin and finally to enter the market. The purpose of this paper is to analyze the synthetic route of epoxidin, determine its technological process and optimize it to meet the requirements of industrial production. Based on the synthetic route of epoxide patent, according to its structural characteristics, three routes were designed and evaluated, and a feasible technological route was determined: using vinylidene chloride as the starting material, nitration, cyclization, nitration and cyclization. The intermediate of nitromethylene was obtained by condensation. The intermediate reacts with 2-dimethoxytetrahydrofuran to hydrolyze succinaldehyde and cyclization to obtain epoxide. In this paper, the synthesis conditions and post-treatment of each reaction in the determined route were optimized, and the effects of various factors on the reaction were discussed, from which the better technological conditions for the synthesis of cycloprozidine were obtained. The cost dropped from 1.69 million yuan / ton to about 870000 yuan / ton. The reaction conditions are mild, the operation is simple, the emission of methionol and the use of excessive ethylenediamine are avoided, which is a more green and environmentally friendly route with the prospect of industrial development.
【学位授予单位】：华东理工大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：TQ453.2
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