4,5-二甲基-1,2-二苯胺的合成工艺改进  

Study on the Synthesis of 4,5-Dimethyl-1,2-dianiline

作　　者：郝艳霞[1] 苏砚溪[2] 

机构地区：[1]石家庄职业技术学院化工系,河北石家庄050081 [2]河北师范大学化学学院,河北石家庄050091

出　　处：《化学世界》2003年第10期547-549,共3页Chemical World

基　　金：河北省教育厅科研基金资助项目(2001233)

摘　　要：以3,4-二甲基苯胺为原料,合成了4,5-二甲基-1,2-二苯胺,产品收率达69%以上。在乙酰化、硝化反应中引入了1,2-二氯乙烷溶剂。用正交实验确定了最佳原料配比:n(3,4-二甲基苯胺)∶n(醋酸酐)∶n(硫酸)=1.00∶1.15∶1.10,硝化反应温度为13°C,反应时间为3.5h,硝化产物收率为90.56%,溶剂回收率95%以上。改进后,每摩尔母体的醋酸酐用量由303g减少至118g,浓硫酸用量由304g减少至108g。4,5Dimethyl1,2dianiline was synthesized with 3,4dimethyl aniline as raw material. The yield of product was over 69%. In the reaction of acetylation and nitration 1,2dichloroethane was used as solvent. The optimal molar ratio of the reactants was 3,4dimethylaniline∶acetic anhydride∶sulfuric acid=1.00∶1.15∶1.10. The nitration temperature was 13°C, and the reaction time was 3.5 h. The yeild of the nitrified product was 90.56%, and the recovery of solvent was over 95%. In this improved method, the consumption of acetic anhydride was reduced from 303 g to 118 g, and the consumption of sulfuric acid was reduced from 304 g to 108 g.

关 键 词：4 5-二甲基-1 2-二苯胺 3 4-二甲基苯胺 乙酰化 硝化 

分 类 号：O625.637[理学—有机化学] TQ246.3[理学—化学]