对乙酰氨基酚琥珀酸酯的合成及其表征分析

本研究以对乙酰氨基酚(APAP)和琥珀酸酐为原料,4-二甲氨基吡啶(DMAP)作催化剂,丙酮作溶剂,经一步反应合成对乙酰氨基酚琥珀酸酯(AP-S);以AP-S产率为指标,采用正交试验设计考察了原料配比、溶媒用量、反应温度、反应时间等因素的影响;分别采用化学鉴定法、熔点测定法、pH测定法、紫外扫描法(UV)、红外扫描法(IR)和高效液相法(HPLC)对AP-S进行鉴定。结果表明,产物表征符合AP-S特征,AP-S最佳合成条件为:琥珀酸酐与APAP摩尔比2∶1,催化剂0.15 g,丙酮30 mL,反应温度60 ℃,反应时间6 h。在优化条件下,AP-S收率可达81.7%。

Study on the Synthesis of Paracetamol Succinate and its Characteristics

Paracetamol succinate(AP-S) was synthesized from paracetamol and succinic anhydride by using 4-dimethylaminopyridine(DMAP) as catalyst and acetone as solvent.AP-S yield was selected as the main index,the synthetic technology was optimized by an orthogonal design including factors such as raw material monomer ratio,solvent dosage,reaction temperature,reaction time and so on.Characteristics of AP-S were identified by chemical identification,pH test,melting point test,IR,UV and HPLC.In result,the features of resultants was consistant with AP-S.The optimized synthetic technology was succinic anhydride and paracetamol monomer ratio 2∶1,catalyst 0.15 g,acetone 30 mL,temperature 60 ℃ and time 6 h,and the yield was 81.7%.