摘要
介绍一种改进的地奥司明的合成方法，以橙皮苷为原料，溶解于吡啶中与碘发生碘代反应，经过脱氢反应制得地奥司明。考察了投料比、反应时间、反应温度、水解条件等影响产品收率和含量的因素，得到最佳反应条件如下：投料比5：1（吡啶：橙皮苷v／w），反应时间10h，反应温度90～95℃，水解pH11，时间1h，温度70℃。得到2种规格的产品，产品I含量为95．82％，收率78．26％；产品Ⅱ含量为90．31％，收率16．43％。该工艺具有生产成本低，工艺稳定，收率和含量高，物耗、能耗显著降低的优点。
This article described the synthesis technology of diosmin. It was prepared from hesperidin by dehydrogenate reaction with iodine in solvent pyridine. The impact of various reaction conditions on the yield and content was studied, such as feed ratio, reaction time, temperature and hydrolysis conditions . The optimum reaction conditions were determined：the feed ratio of pyrdine and hesperidin is 5 ： 1 （v/w） , reaction time 10 h, temperature 90 - 95 ~C The hydrolysis conditions were optimized as follows：pH 11,70 ~C , 1 h. Two special products were got：the yield of 78.26% and the content 95.82% ,the yield of 16.43% and the content of 90.31% respectively. This study has the advantage of low cost and high content and yield.
出处
《实验室研究与探索》
CAS
北大核心
2010年第8期39-41,共3页
Research and Exploration In Laboratory
关键词
橙皮苷
地奥司明
合成
纯化
hesperidin
diosmin
synthesis
purification
