Song Jinglei, Yu Meixuan, Yan Xi, Hao Haijun
College of Chemistry, Beijing Normal University, Beijing, 100875, PR China.
Department of Organic Chemistry, College of Science, Beijing University of Chemical Technology, Beijing, 100029, PR China.
MethodsX. 2020 Apr 25;7:100903. doi: 10.1016/j.mex.2020.100903. eCollection 2020.
We have prepared a kind of new type of flavonoid nitrogen mustard derivatives with broad-spectrum antitumor activity, which have not been reported in the literature. In the process of preparing intermediate (the flavonoid diethanolamine derivatives) of the target compound, we found that the reasonable separation method is silica gel column chromatography with eluent (MeOH/CHCl, 1:40). The experimental results show that the composition of eluent is an important factor to get high yield of the intermediate, which will directly affect the final yield of the target compound. Acetonitrile is the suitable solvent in the reaction system, and the optimized reaction condition is reaction under reflux condition for 48 hours. Several new flavonoid nitrogen mustard derivatives were synthesized with high yield using the above method.•A method for the synthesis of flavonoid nitrogen mustard derivatives was introduced.•The reasonable purification conditions and the optimized reaction time were recommended.
我们制备了一种具有广谱抗肿瘤活性的新型黄酮氮芥衍生物，文献中尚未有相关报道。在制备目标化合物的中间体（黄酮二乙醇胺衍生物）过程中，我们发现合理的分离方法是以甲醇/氯仿（1:40）为洗脱剂的硅胶柱色谱法。实验结果表明，洗脱剂的组成是获得高产率中间体的重要因素，这将直接影响目标化合物的最终产率。乙腈是反应体系中的合适溶剂，优化的反应条件是在回流条件下反应48小时。使用上述方法以高产率合成了几种新型黄酮氮芥衍生物。
•介绍了一种黄酮氮芥衍生物的合成方法。
•推荐了合理的纯化条件和优化的反应时间。
