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作 者:郑怡倩 丁莉莉[1,2] 汪鲁焱 余玉 刘安昌[1,2]
机构地区:[1]武汉工程大学化工与制药学院,湖北武汉430205 [2]绿色化工过程教育部重点实验室(武汉工程大学),湖北武汉430205
出 处:《武汉工程大学学报》2018年第1期23-27,共5页Journal of Wuhan Institute of Technology
摘 要:以丙二酸二乙酯作为起始原料,依次经过氯化、氟化、环合得到3,5-二羟基-4-氟嘧啶,然后与三氯氧磷在回流作用下经过氯化反应,再与邻氯苯酚经过醚化反应得到4-氯-6-(2-氯苯氧基)-5-氟嘧啶,最后与E-(5.6-二氢-[1,4,2]-二噁嗪-3-基)-(2-羟基苯基)-甲酮-O-甲基肟发生醚化反应得到氟嘧菌酯。该合成工艺的总收率为33.2%。产品结构经1H NMR光谱鉴定。该工艺路线具有原料易得、易于控制、收率高等优势,适宜于工业化生产。Using diethyl 2-chloro-malonate as starting material,the 3,5-dihydroxy-4-fluoropyrimidine wassynthesized through chlorination, fluorination, and cyclization reaction, then the 4-Chloro-6-(2-chlorophenoxy)-5-fluoropyrimidine was generated by chlorinating the 3,5-dihydroxy-4-fluoropyrimidine inthe presence of phosphine oxychloride under reflux,and etherifying with o-chlorophenol. The final productfluoxastrobinto was obtained through the reaction of 4-Chloro-6-(2-chlorophenoxy)-5-fluoropyrimidine withE-(5.6-Dihydro-[1,4,2]-dioxizin-3-yl)-(2-hydroxyphenyl)-methanone-O-methyloxime. The structure of theproduct was confirmed by nuclear magnetic spectroscopy. The total yield of this synthetic process was more than 33.2%. Due to the available raw materials,mild reactive conditions and high yields,the developed syntheticroutes is suitable for the large-scale production in industry.
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