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三氟咪啶酰胺关键中间体的合成工艺研究 被引量:1

Synthesis of the Key Intermediates of Triflumidin Amide
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摘要 以丙酮酸乙酯为原料,经过取代反应得到溴代丙酮酸乙酯(F1),优化条件下收率达到94.06%。2,3-二氯-5-(三氟甲基)吡啶经过取代反应得到2-氨基-3-氯-5-(三氟甲基)吡啶(F2),优化条件下收率达到87.12%。F1和F2经过缩合反应得到8-氯-6-(三氟甲基)咪唑并[1,2-A]吡啶-2-羧酸乙酯(F3)。F2和F3经1H NMR确证结构。该制备方法三废少、污染小、收率高,具有工业化应用前景。 Ethyl bromopyruvate(■) was synthesized from ethyl pyruvate through a substitution reactionwith a yield of 94.06% under the optimum conditions. 3-Chloro-5-(trifluoromethyl)pyridin-2-amine(■) was obtained through a substitution reaction of 2,3-dichloro-5-(trifluoromethyl)pyridine in a yield of 87.12%.■ and ■were reacted to give 8-chloro-6-(trifluoromethyl)imidazo[1,2-A]pyridine-2-carboxylate(■). The structures of ■and ■were confirmed by 1H NMR. This preparation method had the advantages including less waste, less pollution and high yield with a prospect of industrial application.
作者 陈羽阳 蒋倩茜 罗晶玲 黄朋勉 CHEN Yu-yang;JIANG Qian-qian;LUO Jing-ling;HUANG Peng-mian(Changsha University of Science and Technology,College of Chemical and Food Engineering,Changsha 410000,China)
出处 《精细化工中间体》 CAS 2021年第2期23-26,共4页 Fine Chemical Intermediates
基金 湖南省教育厅科学研究项目资助(20A019)。
关键词 三氟咪啶酰胺 溴代丙酮酸乙酯 2-氨基-3-氯-5-(三氟甲基)吡啶 8-氯-6-(三氟甲基)咪唑并[1 2-A]吡啶-2-羧酸乙酯 fluazaindolizine ethyl bromopyruvate 3-chloro-5-(trifluoromethyl)pyridin-2-amine ethyl 8-chloro-6-(trifluoromethyl)imidazo[1 2-A]pyridine-2-carboxylate
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