正交试验优化盐酸普鲁卡因中间体的合成工艺

Optimizing of Diethylaminoethyl p-Nitrobenzoate Synthesis by Orthogonal Test

目的采用正交试验法优化盐酸普鲁卡因中间体硝基卡因的直接酯化工艺。方法采用正交设计法的4因素3水平L9(34)试验方案。选择对硝基苯甲酸与N,N-二乙氨基乙醇物质的量比、溶剂二甲苯、反应时间为考察因素。通过直观分析和方差分析确定硝基卡因的合成最佳工艺。结果最佳工艺条件是投料比为1∶1.20,反应时间为7 h,溶剂二甲苯用量为200 m L。结论该合成硝基卡因的方法具有收率高、工艺简单、稳定可行的特点。

Objective to optimize diethylaminoethyl p - nitrobenzoate synthesis by orthogonal test. Methods According to the orthogonal design method. 4 factors and 3 levels were adopted to synthesis of diethylaminoethyl p - nitrobenzoate . Taking the molar ratio of P - nitrobenzoic acid and N, N - diethyl amino ethanol , volume of dimethyl - Benzene solvent , reaction time as investigation factors, to determine the optimum condition of diethylaminoethyl p - nitrobenzoate synthesis through direct viewing analysis and variance analysis. Results The optimal condition were as follows ： the molar ratio of 1 ： 1.20, reaction time of 6 h, volume of dimethyl - Benzene solvent was 200 mL. Conclusion This method has a high yield, the process is simple, stable and practical features.