间硝基苯甲酰亚肼基二硫代碳酸苄酯的合成  

Synthesis of N-(m-nitrobenzoylhydrazono)-S, S'-dibenzyldithiocarbonate

作　　者：陈平生[1] 罗书平[1] 王文静[1] 郑鹛[1] 

机构地区：[1]浙江工业大学化学工程学院,浙江杭州310014

出　　处：《应用化工》2003年第4期44-46,共3页Applied Chemical Industry

摘　　要：以间硝基苯甲酸为原料,经酯化、取代等多步反应,合成间硝基苯甲酰亚肼基二硫代碳酸苄酯,优化了各步反应条件。结果表明,合成间硝基苯甲酰亚肼基二硫代碳酸苄酯的优化条件为:催化剂浓硫酸用量3g/mol,间硝基苯甲酸甲酯与水合肼的摩尔比为1∶1.15,间硝基苯甲酰肼与二硫化碳、氢氧化钾的物质的量比为1∶1.05∶2.0,滴加二硫化碳的温度为0～5℃,亲核取代反应温度为80℃。产品收率77.3%,产物结构通过红外、核磁和气 质联用进行了表征。The synthesis of N(mnitrobenzoylhydrazono)S, S'dibenzyldithiocarbonate by some reactions from mnitrobenzoic acid was studied. The reaction conditions of esterification, substitution reaction and nucleophilic substitution were discussed. The optimum reaction conditions were as follows: the amount of concentrated sulfuric acid which act as the catalyst of esterification was 3 g/mol; the molecular proportion of methyl mnitrobenzoate and hydrazine hydrate was 1∶1.15; the molecular proportion of mnitrobenzoyl hydrazine to carbon bisulfide and sodium hydroxide was 1∶1.05∶2.0; the temperature of droping carbon bisulfide was 0～5 ℃; the nucleophilic substitution reaction proceeded at 80 ℃. The product was over 77.3% yield and was characterized by means of IR,1HNMR and GCMS. 

关 键 词：间硝基苯甲酰亚肼基二硫代碳酸苄酯 间硝基苯甲酰肼 间硝基苯甲酸甲酯 合成 

分 类 号：TQ457.2[化学工程—农药化工]