摘要
以邻硝基甲苯作为初始原料,通过溴化、水解、氧化等步骤制备邻硝基苯甲醛。结果表明,溴化反应中物料配比为:n(邻硝基甲苯)∶n(液溴)=1∶0.45,邻硝基溴苄在80℃条件下,15%(m/m)碳酸钠溶液中水解5 h即可达到99.6%的水解率;氧化反应中,采用二氧六环为溶剂,物料配比为:n(邻硝基苯甲醇)∶n(氢溴酸)∶n(双氧水)=1∶0.23∶1.81时,有较高的转化率与选择性。经多步合成与纯化,该工艺单程总收率41.8%,产品纯度99.6%(HPLC)。
2-Nitrobenzaldehyde was prepared from 2-nitrotoluene via bromination,hydrolysis and oxidation in overall yield of 41.8% with a purity of 99.6%（HPLC）. The reaction conditions were optimized. The molar ratio of 2-nitrotoluene to bromine was 1 to 0.45 in the bromination reaction. 2-Nitrobenzyl bromide was hydrolyzed in solution of sodium carbonate（15%,m / m）for 5 hours. In the oxidation process conducted in dioxane the molar ratio of 2-nitrobenzyl alcohol to hydrobromide to hydrogen peroxide was 1 to 0.23 to 1.81.
出处
《精细化工中间体》
CAS
2013年第5期30-33,共4页
Fine Chemical Intermediates
关键词
邻硝基苯甲醛
工艺
工业化
邻硝基甲苯
2-nitrobenzaldehyde
process
industrialization
2-nitrotoluene
