BTC法合成苯磺酰肼的研究  

Synthesis of benzenesulfonyl hydrazide with bis(trichloromethyl)carbonate

作　　者：刘会君[1] 翁建全[1] 曹耀艳[1] 张红敏[1] 

机构地区：[1]浙江工业大学化学工程与材料学院,浙江杭州310032

出　　处：《浙江工业大学学报》2012年第1期5-7,共3页Journal of Zhejiang University of Technology

基　　金：国家自然科学基金资助项目(30900959);浙江工业大学化学工程与新材料研究生教育创新示范基地项目(2011)

摘　　要：在二氯乙烷溶剂中采用N,N-二甲基甲酰胺作催化剂,苯磺酸钠与双(三氯甲基)碳酸酯(BTC)反应制备苯磺酰氯,然后肼解得到苯磺酰肼.研究了催化剂、溶剂和BTC用量对苯磺酰氯收率的影响,优化条件下氯化反应收率为90.8%;此外,对肼解反应滴加温度和反应温度对苯磺酰肼收率的影响进行了考察.优化条件下,苯磺酰肼两步总收率81.9%,其结构经1 H NMR和IR表征确认.采用BTC代替三氯氧磷作氯化试剂,操作安全,并可避免含磷废水对环境的影响,是一种绿色环保的工艺.Benzenesulfonyl hydrazide was synthesized from benzensulfonyl chloride,which was obtained by the reaction of sodium benzenesulfonate with bis（trichloromethyl）carbonate（BTC） in dichlorethane.The reaction conditions of chlorination,such as catalyst,slovent and the amount of BTC,were investigated.The optimized yield of 90.8% was obtained.In addition,the effects of adding temperature and reaction temperature on hydrazinolysis reaction were also investigated.Under the optimized conditions,the total yield of benzenesulfonyl hydrazide was 81.9%,and the structure of product was confirmed by 1H NMR and IR.It is a green chlorination process with BTC as chlorination reagent instead of POCl3,which has the advantages of safe operation and the avoidance of phosphorus wastewater.

关 键 词：苯磺酰肼 双(三氯甲基)碳酸酯 合成 

分 类 号：TQ247.5[化学工程—有机化工]