偶氮二甲酸二甲酯合成研究  

Studies on Synthesis of Methyl Azodicarboxylate

作　　者：吕硕[1] 陈玉琴[1] 满成娜[1] 

机构地区：[1]山东师范大学化学化工与材料科学学院,山东济南250014

出　　处：《山东化工》2013年第4期5-7,10,共4页Shandong Chemical Industry

摘　　要：研究了以偶氮二甲酰胺为原料,水解生成偶氮二甲酸盐,滴加硫酸二甲酯生成偶氮二甲酸二甲酯的新工艺。对甲基化反应的最佳工艺条件进行了探讨,结果表明:以水作为溶剂,n(硫酸二甲酯):n(偶氮二甲酰胺)=2.4:1,反应温度为55℃,反应时间在3 h,pH值为9～10,收率达到90.9%。改进的合成工艺条件缓和操作简便、合理且可行,提高了产率。The synthesis of methyl azodicarboxylate was studied according to using a new technology that vinyfor AC was used as the main raw material, followed by hydrolyzing, thentthe target product was the reaction withdimethylsulfatedropwise. The optimum condition of ethylation reaction was discussed, the results showed that the yield was up to 90.9% when water was used as solvent, n （dimethylsulfate） ：n （azodicarbonamide） = 2.4 ： 1, the reaction temperature was controlled 55~C, the reaction time was 3 h, and pH 9 - 10, The improved technology was reasonable and feasible because of its mild systhesis condition and simple operation, and gave a high yield.

关 键 词：偶氮二甲酰胺 硫酸二甲酯 偶氮二甲酸二甲酯 

分 类 号：O623.74[理学—有机化学]