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发明授权
CN101774967B 一种制备2,6-二氯-5-氟烟酰乙酸乙酯的方法 有权

一种制备2,6-二氯-5-氟烟酰乙酸乙酯的方法
摘要：
本发明涉及一种制备2，6-二氯-5-氟烟酰乙酸乙酯的方法。以2，6-二氯-5-氟-3-吡啶甲腈为原料生成锌盐中间体3-(2，6-二氯-5-氟-3-吡啶基)-3-亚氨基丙酸乙酯溴化锌盐，然后酸化为亚胺酯中间体3-(2，6-二氯-5-氟-3-吡啶基)-3-亚氨基丙酸乙酯，经酸解制得2，6-二氯-5-氟烟酰乙酸乙酯，特点是其酸化为亚胺酯中间体的温度是0～10℃，pH是2～3，生成的亚胺酯中间体经萃取、蒸馏，分离出不含水的亚胺酯中间体油状液；其酸解是在无水乙醇溶剂中，在20～30℃用氯化氢的无水乙醇溶液或浓硫酸，对不含水的亚胺酯中间体油状液进行酸催化醇解。总收率88～95％，纯度99％，重现性好。
摘要（英）：

The invention relates to a method for preparing 2, 6-dichloro-5-fluorine nicotinoyl ethyl acetate, which comprises the following steps: taking 2, 6-dichloro-5-fluorine-3-pyridine carbonitrile as a raw material, producing a zinc salt intermediate 3-(2, 6-dichloro-5-fluorine-3-pyridyl)-3-imino ethyl propionate zinc bromide, and then acidating the zinc salt intermediate into an imido ester intermediate 3- (2, 6-dichloro-5-fluorine-3-pyridyl)-3-imino ethyl propionate, thus obtaining the 2, 6-dichloro-5-fluorine nicotinoyl ethyl acetate through the acidolysis of the imido ester intermediate. The method is characterized in that the temperature for acidification of the zinc salt intermediate to the imido ester intermediate is 0-10 DEG C and the pH thereof is 2-3, the oily liquid of unhydrous imido ester intermediate can be separated through extracting and distilling the produced imido ester intermediate; the acidolysis of the imido ester intermediate is carried out in absolute ethyl alcohol solvent, and the acid catalyzed alcoholysis of the oily liquid of unhydrous imido ester intermediate is carried out with absolute ethyl alcohol solution of hydrogen chloride or concentrated sulfuric acid under the temperature of 20-30 DEG C. The total yield reaches 88-95 percent, the purity reaches 99 percent, and the invention has good reproducibility.

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