高效除草剂氟草烟仲辛酯合成工艺研究.docVIP

摘  要  氟草烟仲辛酯的化学名称为4-氨基-3，5-二氯-6-氟-2-吡啶氧乙酸（1-甲基庚 酯），熔点56-57，常温下贮存稳定期为两年，高于熔点分解，工业原药为具 有肥皂气味的白色晶体。氟草烟仲辛酯是一种具有内吸传导性除草剂，可用作苗 后茎叶处理，适用于多种作物，如小麦、大麦、玉米、果园等冬季作物，防除多 种恶性杂草愧，如猪秧秧、水花生、田旋花等。 氟草烟仲辛酯产品国内有对其用途和使用方法的研究报道，尚未见其合成方 法的报道；国外对其合成方法的研究较多，主要合成方法有：烷基法、酯交换法、 醇羟基羧酸酯法、氯代硫醇法、甲醇钠法。本论文系统研究了国外文献中关于氟 草烟仲辛酯的合成报道，确定烷基法和酯交换法两条合成工艺对氟草烟仲辛酯工 业化有较好的应用前景，并对烷基法和酯交换法合成工艺参数进行优化。 通过实验建立了氟草烟仲辛酯合成过程中间体和氟草烟仲辛酯的分析方法， 分别优化了烷基法和酯交换法各步反应的工艺条件，得到较佳的结果。烷基化法 先通过酯化反应和碱解反应分别得到中间产物氯乙酸仲辛酯和4-氨基-3，5-二氯 -6-氟-2-吡啶酚钾，再将4-氨基-3，5-二氯-6-氟-2-吡啶酚钾和氯乙酸仲辛酯直接 醚化得到产物氟草烟仲辛酯，粗产物经氢氧化钾水溶液碱洗提纯，产品含量可达 到99.0%以上、收率90.2%；酯交换法是先将4-氨基-3，5-二氯-6-氟-2-吡啶酚钾先 与氯乙酸甲酯醚化合成氟草烟甲酯，再将得到的氟草烟甲酯与仲辛醇在钛酸丁酯 催化下发生酯交换反应得到产物氟草烟仲辛酯，产品总收率可达91.1%，纯度 98.7%。  关键词：  氟草烟仲辛酯； 合成； 酯交换 I Abstract Fluroxypyr 1-methylheptyl ester breathing the chemical name for ((4-Amino-3,5-dichloro-6-fluoro-2-pyridinyl)oxy)-acetic acid 1-methylheptyl ester, the melting point 56-57 ℃, storage and stability at room temperature for two years, higher than the melting point of decomposition, the drug industry as a soap smell of white crystals. Fluroxypyr 1-methylheptyl ester is a kind of absorption in the conduction of the herbicide, stems and leaves can be used as Miaohou treatment, apply to a variety of crops such as wheat, barley, corn, orchards and other winter crops, control of weeds in a variety of malignant Kui, Yang Yang such as pigs, water peanuts, field bindweed, and so on. Fluroxypyr 1-methylheptyl ester product use and domestic use of its research reports, synthesis methods have not yet are reflected in its reports; abroad to study the synthesis of more, mainly synthetic methods are: alkyl, transesterification, Alcohol hydroxy-carboxylate, chlorinated mercaptan, methanol sodium law. This paper system of the foreign literature on the Fluroxypyr 1-methylheptyl ester Synthesis of reports, and identified Alkylation and transesterification methods of synthesis of Fluroxypyr 1-methylheptyl ester industrialization has good prospect and Alkylation and Ester exchange of techni