一步法合成N-(1-乙基丙基)-3,4-二甲基苯胺  

One Step Synthesis for Perparation of N-(1-ethylpropyl)-3,4-dimethylaniline

作　　者：徐振元[1] 严新焕[1] 许丹倩[1] 张国富[1] 楼芝英[1] 

机构地区：[1]浙江工业大学化工学院,浙江杭州310014

出　　处：《高校化学工程学报》2002年第1期75-78,共4页Journal of Chemical Engineering of Chinese Universities

基　　金：浙江省重大科技攻关项目(001101075)

摘　　要：以自制的Pd-Pt/C为加氢催化剂,有机酸为助催化剂,3,4-二甲基硝基苯和3-戊酮为原料,通过硝基加氢、酮胺加成、脱水与碳氮双键加氢一系列反应一步法合成了N-(1-乙基丙基)-3,4-二甲基苯胺。考察了不同加氢催化剂、助催化剂和反应温度对该反应的影响;在较佳的反应工艺条件下,四步反应的总收率达98.6%,比文献值收率提高10%。In order to improve the reaction for preparation of N-(1-ethylpropyl)-3,4-dimethylaniline, one step synthesis reaction and reaction mechanism were proposed and 3,4-dimethylnitrobenzene was selected as the start material. Several factors such as hydrogenation catalyst, promotion acid catalyst and reaction temperature etc. were considerd and tested. The Pt-Pd/C bimetal hydrogenation catalyst was proved to be more efficient in this reaction than Pt/C catalyst. Middle acidity organic acid which has lower solubility in water can be selected as promotion catalyst. Much more intermediate compounds may exist when the reaction temperature is lower than 80℃, and more byproducts may be produced when temperature is higher than 120℃. Therefore the best reaction temperature was ranged from 80℃ to 120℃. At the suitable reaction conditions such as using Pt-Pd/C as hydrogenation catalyst; benzenesulfonic acid as promotion acid catalyst; reaction temperature: 100℃; hydrogen pressure: 1.2MPa; 3-pentanone: 3,4-dimethylnitrobenzene (molar ration)=2:1; 3,4-dimethylnitrobenzene:catalyst (weight ration)=100:1, the total yield reached to 98.6% and that in about 10% higher than ordinary reaction for preparation of N-(1-ethylpropyl)-3,4-dimethylaniline.

关 键 词：3 4-二甲基硝基苯 3-戊酮 催化加氢 合成 N-(1-2乙基丙基)-3 4-二甲基苯胺 除草剂 中间体 二甲戊乐灵 

分 类 号：TQ457.2[化学工程—农药化工]