| 周采菊,高红刚,郭永恩,李爱华,刘帅,王保国.藤黄酸类成分的硅胶干柱层析法分离及其酰胺新实体的合成[J].济宁医学院学报,2021,44(4):234-237 |
| 藤黄酸类成分的硅胶干柱层析法分离及其酰胺新实体的合成 |
| Purification of gambogic cacids by silica gel dry column chromatography and synthesis of their new amide entities |
| 投稿时间：2021-02-15 |
| DOI：10.3969/j.issn.1000-9760.2021.04.002 |
| 中文关键词: 藤黄酸;新藤黄酸;N-芳基酰胺;N-烷基酰胺;合成;分离 |
| 英文关键词: Gambogic acid;N-aryl amide;N-alkyl amide;Synthesis;Purification. |
| 基金项目:山东省科技发展计划项目（2013jsf11910）；济宁市医药科技发展项目（2012jnjc04） |
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| 中文摘要: |
| 目的 探讨从藤黄中提取分离藤黄酸（GA）、新藤黄酸（GNA）的实验技术及其酰胺新实体的合成。方法 藤黄丙酮提取物中分离出藤黄酸吡啶盐的母液浸膏与200目硅胶均匀混合后干法上样，硅胶H干柱逆流梯度层析分离出GA、GNA，N，N’-二异丙基碳二亚胺法催化合成它们的N-芳基和N-烷基酰胺。结果 较高效分离出GA、GNA，温和制备了N-[2-（N’，N’-二甲氨基）乙基]藤黄酰胺、N-（3-氯-4-氟苯基）新藤黄酰胺和N-（3-氯-4-氟苯基）藤黄酰胺3种酰胺新实体。结论 本实验所建立的GA、GNA干柱逆流层析分离及其酰胺化方法操作简便、温和、重现性好。 |
| 英文摘要: |
| Objective The extraction of gambogic acid (GA) and gambogenic acid (GNA) from gamboge and purification by dry column chromatography, and synthesis of their new amide entities were emphasized.Methods Dried powdered residue from gamboge extract left after GA pyridine salt precipitated was mixed with 200 mesh silica gel, put under silica gel H and chromatographed by gradient eluent.N, N'-diisopropyl carbodiimide (DIC) catalyzed their amidation with aliphatic amine and aromatic amine.Results GA and GNA were purified in high purity and good recovery yields, and three new entities of their amides were mildly synthesized.Conclusion GA and GNA purification by silica gel H dry column chromatography is easily operated in good reproducibility. |
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