双氧水介导制备对硝基苯甲酸乙酯的初步研究

Study on Mediate Preparation of Hydrogen Peroxide in Synthesis of Ethyl-P-Nitrobenzoate

目的:探讨双氧水催化合成对硝基苯甲酸乙酯的可行性,并考察了反应物的摩尔比、催化剂用量、反应温度及反应时间对产物收率的影响。方法:分别采用单因素设计实验与正交设计实验,分析比较这两种方法的最佳反应条件。采用数字熔点仪测定样品的熔点;用GC112A型气相色谱仪测定了产物的纯度;用傅里叶变换红外光谱仪测定产物的结构。结果:双氧水可以作为合成对硝基苯甲酸乙酯的催化剂。综合分析可知:当无水乙醇和对硝基苯甲酸的摩尔比为4∶1,催化剂含量为10%,反应温度为80℃,反应时间为2.5-3h时酯化产率可达到最高值。结论:双氧水催化对硝基苯甲酸、无水乙醇合成对硝基苯甲酸乙酯的效率较高,产品纯度高,环境污染小,不失为一种新的合成方法。

Objective： To investigate the feasibility of the synthesis of Ethyl-p-Nitrobenzoate catalysed by Hydrogen Peroxide. We study the effects of the actor mole ratio, catalyst dosage, reaction temperature, and reation time on the esterification rate. Method： In order to obtain the optimization reaction condition, single factor experiments were performed, and then based on the results of these single factor experiments, the orthogonal design experiments were performed. The results of these experiments were analysised. The meltiong point of the product were surveyed using number melting point equipment, and the purity of the product was evaluated using the GC112A model gas chromatograph, and the structure of the product was determined using the Fourier transfom. Results： Hydrogen peroxide is a good catalyst in the synthesis of Ethyl-p-Nitrobenzoate reaction. The results showed the optimal yield was obtained when the product was prepared at 80℃ for 2.5-3h with the 4：1 molar ratio of the reactants [n （dehydrated alcohol）： n （p-nitrobenzoic acid）]. Conclusion： In the synthesis of Ethyl-p-Nitrobenzoate reaction, the Hydrogen peroxide can be used as a good catalyst since it exhibits very high level of the catalysis rate and highly purified product yield.