摘要
硫氰酸红霉素、三乙胺、盐酸羟胺"一锅法"合成红霉素A肟硫氰酸盐,再用NaOH溶液中和、乙醇/水体系重结晶得标题化合物。产品用熔点测定、元素分析、IR和1HNMR进行了表征。探索了反应条件对产品收率和纯度的影响。在优化条件下,产品的总收率为85.6%,纯度>97.8%(HPLC)。与其他工艺相比,生产成本可明显降低。
( E)-erythromycin A oxime was synthesized in one pot by the oximation reaction using erythromycin thiocyanate, triethylamine and hydroxyamine hydrochloride as the starting materials, followed by neutralization with NaOH solution and recrystallization in the ethanol/water system. The product structure was confirmed by melting point determination, elementary analysis. IR spectrometry and ^1HNMR spectrometry. Effects of reaction conditions on the product yield and purity were investigated. The product yield reached 85.6 % and the purity of product obtained under optimum reaction conditions exceeded 97.8% (as analyzed by HPLC). The production cost was much lower as compared to other synthetic processes.
出处
《化学试剂》
CAS
CSCD
北大核心
2009年第7期565-567,570,共4页
Chemical Reagents