2-氯-5-氯甲基吡啶的绿色合成工艺  

A Green Process for the Synthesis of 2-Chloro-5-chloromethyl Pyridine

作　　者：杜友兴 何立 DU You-xing;HE Li(Shanghai Chemspec Corporation,Shanghai 200331,China)

机构地区：[1]上海康鹏科技股份有限公司

出　　处：《农药》2019年第12期878-881,884,共5页Agrochemicals

摘　　要：[目的]2-氯-5-氯甲基吡啶的绿色合成新工艺研究。[方法]开发了以2-氯-2-氯甲基-4-氰基丁醛为原料,三聚氯氰作为环合试剂,合成2-氯-5-氯甲基吡啶的新工艺。研究了环合反应机理,通过单因素试验探讨了温度、物料配比、滴加方式等因素对反应收率的影响。通过正交试验研究了环合滤渣氰尿酸回收制备三氯异氰尿酸的工艺条件。[结果]反应外标收率达86.4%,并副产三氯异氰尿酸。[结论]工艺过程清洁、绿色环保,适合工业化生产。[Aims] The paper aims to study a new green synthesis process of 2-chloro-5-chloromethylpyridine.[Methods] 2-Chloro-5-chloromethyl pyridine was synthesized with 2-chloro-2-chloromethyl-4-cyanbutyraldehyde as starting material and cyanuric chloride as cyclization reagent. The mechanism of cyclization reaction was studied, and the effects of temperature, material ratio and dropping method on the yield were also discussed through single factor experiments. The technological conditions for the preparation of trichloroisocyanuric acid from cyanuric acid recovery from cyclic filter residue were investigated by orthogonal experiment. [Results] The yield of cyclization reaction was 86.4%, and by-product trichloroisocyanuric acid was obtained. [Conclusions] The process is clean, green and environmentally friendly, and suitable for industrial production.

关 键 词：2-氯-5-氯甲基吡啶 三聚氯氰 环合反应 氰尿酸 三氯异氰尿酸 合成 

分 类 号：TQ460.3[化学工程—制药化工]