丙硫菌唑的合成工艺优化  

Synthesis Process Optimization on Prothioconazole

作　　者：余波[1] 

机构地区：[1]绵阳职业技术学院,四川绵阳621000

出　　处：《农药》2017年第2期105-107,共3页Agrochemicals

摘　　要：[目的]以2-(1-氯环丙基)-3-氯-1-(2-氯苯基)-2-丙醇为原料,通过肼解成盐、环合、氧化反应制得丙硫菌唑,开发丙硫菌唑合成的简便清洁工艺方法。研究肼化合物在多种溶剂中的稳定性,物料配比对环合反应的影响及丙硫菌唑合成氧化剂的筛选。[方法]经反应工艺条件优化,以乙酸乙酯为溶剂制备肼化合物盐酸盐,投料1.2 eq甲醛水溶液和1.5 eq硫氰酸钠完成环合反应,在0.1 eq三氯化铁催化下进行氧化反应。[结果]粗品经重结晶后得到灰白色固体丙硫菌唑。3步反应产品总收率56.2%,液相含量为97.5%。[Aims] Prothioconazole was synthesized from 1-chloro-2-（1-chlorocyclopropyl）-3-（2-chlorophenyl）propan- 2-ol v/a hydrazinolysis reaction, cyclization and oxidation reaction. This study aims to provide an easy and clean preparation method of prothiconazole by exploring the stability of hydrazine compounds in a wide variety of solvents and the influence of material ratio on cyclization reaction and screening oxidants. [Methods] Under the optimal reaction condition, hydrazine compounds were obtained in its salt form by taking ethyl acetate as the solvent, formaldehyde（1.2 eq） and sodium thiocyanate（1.5 eq） were applied to complete the cyclization reaction, and the product prothioconazole was synthesized v/a 0.1 eq ferric trichloride as catalyst. [Restults] The overall yield of prothioeonazole was 56.2%, and the purity of the product was 97.5%.

关 键 词：丙硫菌唑 肼解反应 环合反应 氧化反应 

分 类 号：TQ455.4[化学工程—农药化工]