摘要
以苯甲醇和二正丙胺为原料,以水为溶剂,在绿色氧化剂双氧水、TCCA、TCT氧化催化下合成N,N-二正丙基苯甲酰胺,用正交设计法优化合成工艺,确定最佳工艺条件为反应温度为75℃,反应时间为10 h,醇胺摩尔比为1∶2,H_2O_2用量为200%(mol),n(TCCA)∶n(TCT)=4∶1,N,N-二正丙基苯甲酰胺产率达到75.12%,经过~1H-NMR和^(13)C-NMR确定其结构。改进后的工艺反应条件温和,操作安全简便,符合环境友好化学的发展方向,是一条切实可行的绿色合成工艺路线。
N,N-di-n-propyl benzamide was synthesized with benzyl alcohol and di-n-propyl amine as raw material and water as solvent,and hydrogen peroxide, TCCA, TCT as oxidation catalysis. Technological condition was obtained with orthogonal design. After optimization, the best reaction conditions were as following： reaction temperature is 75 ~C, reaction time is 10 h, the molar ratio of benzyl alcohol and di-n-propyl amine is 1 ： 2, the usage of H202 is 200 %（mol）, n（TCCA） ： n（TCT）is 4 ： 1. The yield of product reached 75.12 %. The target compound was confirmed byIH-NMR and 13C-NMR. The improved and optimized synthesis has more advantages such as mild reaction condition, technique is simple and safe. The developing direction, which is according with environmentally friendly chemistry is a feasible green synthetic route.
出处
《广东化工》
CAS
2016年第11期15-16,共2页
Guangdong Chemical Industry
基金
海南医学院大学生创新性实验项目(HYCX2014058)
关键词
苯甲醇
二正丙胺
N
N-二正丙基苯甲酰胺
正交设计
合成
benzyl alcohol： di-n-propyl amine： N,N-di-n-propyl benzamide： orthogonal design： synthesis
