无水溶剂法合成4-甲氧基苯甲醛的新工艺研究  

A New Process of Synthesizing 4-Methoxybenzaldehyde in Anhydrous Solvent

作　　者：徐保明[1] 付松[1] 李龙腾[1] 陈华[1] 廖帅[1] 吴伟冰[1] 刘欢[1] 

机构地区：[1]湖北工业大学化学与环境工程学院,湖北武汉430068

出　　处：《化学世界》2011年第3期162-165,共4页Chemical World

基　　金：科技部科技人员服务企业项目(2009GJD10016);湖北省教育厅产学研重大项目(CXY2009A010)

摘　　要：研究了以4-羟基苯甲醛和硫酸二甲酯为原料在无水溶剂中合成4-甲氧基苯甲醛的工艺。考察了不同溶剂,加料方式,脱水方式,投料比,反应温度和反应时间诸因素对产物4-甲氧基苯甲醛收率的影响。结果表明:当投料比为n(对羟基苯甲醛):n(硫酸二甲酯):n(无水复合钾盐)=1∶0.67∶0.65,以极性有机物DMF为溶剂,反应温度为150°C,特殊回流脱水方式,反应时间为4h时,产品经过滤,减压蒸馏得无色透明的4-甲氧基苯甲醛液体,收率可达98%以上。A synthesis method of 4-methoxybenzaldehyde by reacting 4-hydroxybenzaldehyde with dimethyl sulfate in anhydrous solvent was studied.The effects of reaction conditions such as different solvents,feeding methods and dehydration ways,molar ratio of raw materials,reaction temperature and reaction time on the yield of 4-methoxybenzaldehyde were investigated.The results showed that the optimum conditions were as follows： n（4-hydroxybenzaldehyde）：n（dimethyl sulfate）：n（anhydrous compound sylvite） =1∶0.67∶0.65,solvent DMF,reaction temperature 150℃,special reflux dehydration and reaction time 4 h.After filtration and reduced pressure distillation,the colourless and transparent liquid of 4methoxybenzaldehyde was obtained,and the yield was over 98%.

关 键 词：4-甲氧基苯甲醛 4-羟基苯甲醛 硫酸二甲酯 合成 

分 类 号：TQ244.1[化学工程—有机化工]