9-氧-2-溴乙基小檗碱,是与贝特类化合物或其它结构类型化合物相结合形成具有降脂降糖等作用药物的关键中间体。本文以小檗碱为原料合成小檗红碱,再将小檗红碱与1,2-二溴乙烷在微波辐射下合成9-氧-2-溴乙基小檗碱。考察了微波功率、反应时间、1,2-二溴乙烷用量、反应温度对于产率的影响。产物纯度和结构经LC-MS和NMR确定,得出最佳合成工艺条件:微波功率500 W、反应时间30 min、小檗红碱与1,2-二溴乙烷用量比1:10 (g)、反应温度70℃。与传统加热方法相比,微波辅助合成可大幅度提升产率并缩短反应时间。
In this paper, berberine was used as raw material to synthesize berberrubine. The reaction of berberrubine and 1,2-dibromoethane with microwave irradiation was carried out to synthesize 9-O-2-bromoethylberberine. The different yields effected with microwave power, reaction time, amount of 1,2-dibromoethane and reaction temperature were investigated. The purity and struc-ture of the product were determined by LC-MS, NMR. The optimum conditions were shown: mi-crowave power 500 W, reaction time 30 min, ratio of berberrubine to 1,2-dibromoethane 1:10 (g), the reaction temperature was 70℃. Compared with the traditional heating method, the yield has increased and the reaction time has decreased with microwave irradiation.
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