氟嘧菌酯的清洁合成工艺

Clean Technology for Synthesis of Fluoxastrobin

[目的]对氟嘧菌酯合成工艺进行清洁化研究。[方法]开发了以4,6-二羟基-5-氟嘧啶为原料,硫酰氟为氟化试剂,“一步法”合成4,5,6-三氟嘧啶的新工艺。4,5,6-三氟嘧啶再与邻氯苯酚和3-[1-(2-羟基苯基)-1-(甲氧亚氨基)-甲基]-5,6-二氢-1,4,2-二嗪经2步醚化反应合成了氟嘧菌酯。[结果]3步反应总收率70.6%,避免了含磷废水排放,并副产氟化钠和氯化钾。[结论]工艺过程清洁、绿色环保、成本低廉,适合工业化生产。

[Aims]This paper aims to study a clean process for synthesis of fluoxastrobin.[Methods]A new one-step process for synthesis of 4,5,6-trifluoropyrimidine was developed with 4,6-dihydroxy-5-fluoropyrimidine as the raw material and sulfuryl fluoride as fluorination reagent.Fluoxastrobin was then synthesized by etherification reaction of 4,5,6-trifluorpyrimidine with O-chlorophenol and 3-[1-(2-hydroxyphenyl)-1-(methoxyimino)-methyl]-5,6-dihydro-1,4,2-dioxin in two steps.[Results]The total yield of the three-step is 70.6%,which avoids the discharge of wastewater containing phosphorus and by-products of sodium fluoride and potassium chloride were received.[Conclusions]The process is clean,environmental friendly with low cost,which is suitable for industrial production.