4-氯-2-氰基-5-(4’-甲基苯基)咪唑的合成工艺优化  

Synthesis of 4-Chloro-2-cyano-5-(4’-methylphenyl)-imidazole

作　　者：王涛 WANG Tao(Shanghai Shengnong Pesticide Co.,Ltd.,Shanghai 201108,China)

机构地区：[1]上海生农生化制品股份有限公司,上海201108

出　　处：《精细化工中间体》2020年第6期32-36,共5页Fine Chemical Intermediates

摘　　要：以2,2-二氯-4’-甲基苯基乙酮为主要原料,与羟胺盐先形成单肟化物,一锅法与40%乙二醛水溶液进行关环反应,得到1-羟基-4-(4’-甲基苯基)-2-甲肟基咪唑-3-氧化物,然后该氧化物先在氯化亚砜的参与下,进行脱水反应得到氰基化物,一锅法再在二氯化硫的参与下进行氯化反应得到4-氯-2-氰基-5-(4’-甲基苯基)咪唑。研究了物料配比、反应温度、反应时间等影响因素,优化后4-氯-2-氰基-5-(4’-甲基苯基)咪唑的总收率达80.5%。该合成方法原料廉价易得,收率高,反应过程简单。1-Hydroxy-4-(4’-methylphenyl)-2-oxyiminomethylimidazole-3-oxide was synthesized using 2,2-dichloro-4’-methyl acetophenone as the starting material followed a series reactions including oxime formation with hydroxylamine salt and cyclization with 40%aqueous solution of glyoxal.And the 4-Chloro-2-cyano-5-(4’-methylphenyl)-imidazole was obtained using the Oxide through reactions including dehydration with thionyl chloride and then chlorination with sulfur dichloride.The effect of material ratio,reaction temperature and reaction time was discussed,and the total yield was 80.5%under the optimized condition.This new synthetic method had the advantages including commercialized raw materials,high yield and simple process.

关 键 词：氰霜唑 4-氯-2-氰基-5-(4’-甲基苯基)咪唑 合成 

分 类 号：TQ460.6[化学工程—制药化工]