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目的采用正交试验法优化硝基卡因的直接酯化工艺。方法以对硝基苯甲酸和N,N-二乙氨基乙醇为原料,通过直接酯化法合成硝基卡因,选择反应的催化剂、溶剂、投料比、时间为考察因素,采用L9(34)正交试验确定硝基卡因的直接酯化法最佳工艺。结果最佳工艺条件是催化剂为甲酸,溶剂为二甲苯,投料比为1∶1.10,反应时间为6 h。最佳工艺条件下的合成收率为98.17%,硝基卡因的质量分数为99.40%。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 the direct esterification of nitrocarbin by orthogonal test. Methods Nitrobaccatin was synthesized by direct esterification using p-nitrobenzoic acid and N, N-diethylaminoethanol as raw materials. The catalyst, solvent, feed ratio and time were selected as the investigation factors. L9 (34) Orthogonal test to determine the optimal process of direct esterification of nitrocaine. Results The optimum conditions were as follows: the catalyst was formic acid, the solvent was xylene, the feed ratio was 1: 1.10 and the reaction time was 6 h. Under the optimal conditions, the yield was 98.17% and the mass fraction of nitrocaine was 99.40%. Conclusion The method of synthesizing nitrocaine has the characteristics of high yield, simple process, stable and feasible.