4-吡咯烷基吡啶催化合成贝诺酯工艺研究

Study on Catalytic Synthesis of Benorilate with 4-Pyrrolidinopyridine

采用新型催化剂4-吡咯烷基吡啶(4-Pyrrolidinopyridine)催化合成贝诺酯。通过实验探究了反应温度、反应时间、原料比例、催化剂种类及用量对目标物产率的影响,并通过均匀试验设计法优化合成条件,寻找最优工艺。合成产物通过红外光谱法(IR)以及拉曼光谱法(Raman)检测分析。其所得最佳工艺条件为:m(4-Pyrrolidinopyridine)∶m(阿司匹林)(%)=6,n(阿司匹林)∶n(二环己基碳二亚胺)=1.0844,V(丙酮)=40 mL,T=50℃,t=2h。根据均匀试验结果对所得最佳工艺进行3次平行实验,平行实验的平均产率为50.42%。实验结果表明,本合成方法与参考文献相比,操作过程简单,反应时间短,反应温度容易满足且易控制,为贝诺酯的合成提供了新的催化方法。

Benorilate was synthesized using a new catalyst 4-pyrrole alkyl pyridine （4-Pyrrolidinopyridine）. The effects of reaction temperature, reaction time, raw material ratio, catalyst type and dosage on the target yield were investigated, and the synthetic conditions were optimized by the uniform test design method. The synthetic products were identified by IR and Raman. The optimum technological conditions were： m（4-Pyrrolidinopyridine）∶m（Aspirin）（%）=6, n（Aspirin）∶n（DCC）=1.0844, V（Acetone）=40 mL, T=50 ℃, t=2.5 h. According to the results of the uniform test, the optimum process was carried out three parallel experiments with an average yield of 50.42 %. The experimental results show that compared with the reference, the synthesis method has a simple operation process, a short reaction time, a reaction temperature that is easy to meet and easy to control, and provides a new catalytic method for the synthesis of the benorilate.