Isolation and characterization of related impurities in 24-epibrassinolide |
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| Authors: | Hongli Chen Yuanchao Li Biao Jiang |
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| Affiliation: | a Shanghai Institute of Materia Medica, Chinese Academy of Sciences, 555 Road Zu Chong Zhi, Zhangjiang Hi-Tech Park, Shanghai 201203, PR China
b Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, 354 Road Fengling, Shanghai 200032, PR China |
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| Abstract: | Two extra-hydroxylated analogs of 24-epibrassinolide (2), 17-hydroxy-24-epibrassinolide (4), 25-hydroxy-24-epibrassinolide (5), and two oxo-analogs of 24-epibrassinolide 22-oxo-23S-24-epibrassinolide (6), 22R-23-oxo-24-epibrassinolide (7) as impurities were isolated and identified from the initial material [purity: 2 and its 22S, 23S-isomer (3) >95%] by using various chromatographic methods and repeated crystallization. Among them, compound 4 and compound 6 were first reported. Their structures were established by spectrometric analysis and X-ray crystallography study. Formation of mixed crystals of 6 and 7 in the crystallization process was postulated and further confirmed. |
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| Keywords: | 24-Epibrassinolide Extra-hydroxylated analogs Oxo-analogs Mixed crystals |
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