摘要
目的:通过Erlenmeyer-Plchl反应制备药物合成的重要中间体3,4,5-三甲氧基苯乙酸。方法:在醋酸、醋酐和醋酸钠存在的条件下,将3,4,5-三甲氧基苯甲醛与马尿酸缩合,得到二氢噁唑酮中间体,再经氢氧化钠水解、过氧化氢氧化得到3,4,5-三甲氧基苯乙酸。结果:所得产物经红外光谱、核磁共振氢谱和质谱确证;总收率约为58%。结论:本方法路线短,原料易得,操作简单,避免了剧毒试剂的使用,更适于工业化生产。
[Abstract] Objective： To synthesize 3, 4, 5-trimethoxyphenyl acetic acid, an important drug interme- diate, by Edenmeyer-Pl^chl reaction. Methods： 3, 4, 5-trimethoxyphenyl acetic acid was synthesized from 3,4, 5-trimethoxybenzaldehyde by condensation with hippuric acid in the presence of acetic anhydride, acetic acid and sodium acetate, followed by alkaline hydrolysis and n202 oxidation. Results： The structure of 3, 4, 5-trimethoxyphenyl acetic acid was confirmed by IR, 1H-NMR and MS. The overall yield was 58%. Conclusion： The synthetic process is short and the raw materials are easy to obtain. Furthermore, the method is simple, avoiding the use of highly toxic reagents. It is suitable for the industrial production.
出处
《药学进展》
CAS
2013年第6期280-283,共4页
Progress in Pharmaceutical Sciences
