两步法合成间硝基苯甲醛  

Two Step Synthesis of m-Nitrobenzaldehyde

作　　者：朱燕[1] 吴广文[1] 黄艳刚[1] 吴浩[1] 虞祺[1] 魏成林[1] 丁敦敦[1] 

机构地区：[1]武汉工程大学湖北省新型反应器与绿色化学工艺重点实验室,湖北武汉430074

出　　处：《精细化工》2011年第2期201-204,共4页Fine Chemicals

摘　　要：间硝基甲苯与双氧水、氢溴酸在AIBN作用下,生成间硝基一溴苄和二溴苄,再经DMSO、二甲胺氧化水解生成间硝基苯甲醛。研究了溴化、氧化水解反应的影响因素,优化了反应条件。结果表明,溴化反应较佳的条件为:溴化温度60℃,溴化时间4 h,n(间硝基甲苯)∶n(氢溴酸)∶n(双氧水)=1∶2.5∶2.5,AIBN用量0.8 g;氧化水解反应较佳的条件为:氧化温度105℃,保温时间8 h,水解温度60℃,水解时间1 h。在该条件下,间硝基苯甲醛收率达58.6%,色谱纯度达99.1%。通过IR和1HNMR对产物结构进行了表征。m-Nitrobenzyl bromide and 1-（dibromomethyl）-3-nitrobenzene,which were prepared with m-nitrotoluene,hydrogen peroxide and hydrobromic acid over AIBN,was oxided and hydrolyzed by DMSO and dimethylamine to produce m-nitrobenzaldehyde.Factors influencing bromination,hydrolysis and oxidization were investigated.The yield and purity of m-nitrobenzaldehyde are 58.6% and 99.1% respectively under the optimal bromination conditions：bromination temperature 60 ℃,bromination time 4 h,n（m-nitrotoluene）∶ n（HBr）∶ n（H2O2）=1∶ 2.5∶ 2.5,the amount of AIBN 0.8 g,and oxidization-hydrolysis conditions：oxidization temperature 105 ℃,heat preservation time 8 h,hydrolysis temperature 60 ℃,hydrolysis time 1 h.The structure of the product was identified by IR and ^1HNMR.

关 键 词：间硝基甲苯 间硝基苯甲醛 溴化 氧化水解 二甲胺 精细化工中间体 

分 类 号：TQ226.14[化学工程—有机化工] TQ207