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.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2011年第2期201-204,共4页
Fine Chemicals
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
m-nitrotoluene； m-nitrobenzaldehyde； bromination； oxidization and hydrolysis； dimethylamine； fine chemical intermediates
