杀菌剂噁醚唑合成工艺研究

Technical Study on Synthesis of Fungicide Difenoconazole

研究了杀菌剂噁醚唑的合成工艺。以苯醚酮为起始原料,经缩酮环化反应、溴代反应、亲核取代反应和粗品精制制得噁醚唑纯品。对各步反应的工艺条件进行优化改进,实验表明,当苯醚酮与1,2-丙二醇的摩尔比为1∶1.35,缩酮与溴的摩尔比为1∶1.30,溴代缩酮与1,2,4-三唑钠的摩尔比为1∶1.25,缩合温度为140℃时,噁醚唑总收率可以高达83%以上,产品纯度达到98%。

Technology on synthesis of fungicide difenoconazole was researched.Difenoconazole was prepared with 2-chloro-4-（4-chlorophenoxy）acetophenone as raw material by ketal cyclization,bromo-reaction,nucleophilic substitution reaction and purification.The each reaction conditions were optimized.The total yield of difenoconazole was more than 83% with purity of 98% when the molar ratio of 2-chloro-4-（4-chlorophenoxy）acetophenone and 1,2-propanediol was 1：1.35,the molar ratio of ketal and bromine was 1：1.30,the molar ratio of bromo-ketal and 1,2,4-triazolylsodium was 1：1.25,meanwhile,the temperature for condensation reaction was 140 ℃.