环戊噻嗪的合成工艺改进

摘要

Cyclopenthiazide was synthesized from cyclopentyl bromide and diethyl malonate by condensation, alkaline hydrolysis, decarboxylation, reduction, oxidation, and cyclization reaction. Chemical structure of the product was comfirmed by nuclear magnetic resonance spectros-copy (1 H NMR) and mass spectrometry (MS) , and its purity was determined based on normalization of high-performance liquid chromatography (HPLC). It was found that target product was obtained at a total yield of 25.5%, and it purity was as much as 99.4 %. The process after being modified is suitable for industrial production owing to its advantages of convenient operation and stabilized process conditions.%以溴代环戊烷和丙二酸二乙酯为起始原料,经缩合、水解、脱羧、还原、氧化、环合六个步骤合成了目标化合物环戊噻嗪；所得产物结构经核磁共振氢谱和质谱确证,产物纯度经高效液相色谱(HPLC)归一化法测定.结果表明,目标产物总收率可达25.5％,纯度为99.4％；经过改进的工艺条件稳定,操作简便,收率明显提高,适合于工业化生产.