目的 采用正交試驗(yàn)法優(yōu)化硝基卡因的直接酯化工藝。方法 以對硝基苯甲酸和N,N-二乙氨基乙醇為原料，通過直接酯化法合成硝基卡因，選擇反應(yīng)的催化劑、溶劑、投料比、時(shí)間為考察因素，采用L9(34)正交試驗(yàn)確定硝基卡因的直接酯化法最佳工藝。結(jié)果 最佳工藝條件是催化劑為甲酸，溶劑為二甲苯，投料比為1∶1.10，反應(yīng)時(shí)間為6 h。最佳工藝條件下的合成收率為98.17%，硝基卡因的質(zhì)量分?jǐn)?shù)為99.40%。結(jié)論 該合成硝基卡因的方法具有收率高、工藝簡單、穩(wěn)定可行的特點(diǎn)。

Objective To optimize the direct esterification prochyl p-nitrobenzoate by orthogonal test. Methods P-nitrobenzoic acid and N,N-diethyl amino ethanol were used as starting materials to synthesize the target compound by direct esterification process. Taking catalyst, solvent, the molar ratio of starting materials and reaction time as investigation factors, the best direct esterification process of diethylaminoethyl p-nitrobenzoate was determined by L9(34) orthogonal test. Results The optimal direct esterification process conditions were as follows: catalyst of formic acid, solvent of xylene, the molar ratio of 1∶1.10, and reaction time of 6 h. The yield of the optimal direct esterification process was 98.17%, and the purity of diethylaminoethyl p-nitrobenzoate was 99.40%. Conclusion The optimal direct esterification process for p-nitrobenzoate has the characteristics of high yield, simple process, stable and feasible.

北京中醫(yī)藥大學(xué)校級課題（2013-JYBZZ-JS-033）