| 3,3,17,17-亚乙二氧基-7-羰基-雄烯二酮的合成研究 |
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| 引用本文： | 陈韶蕊.3,3,17,17-亚乙二氧基-7-羰基-雄烯二酮的合成研究[J].河北工业科技,2012,29(6):370-372,375. |
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| 作者姓名： | 陈韶蕊 |
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| 作者单位： | 河北科技大学理学院,河北石家庄,050018 |
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| 摘 要： | 以雄烯二酮为原料,经3,17位亚乙二氧基化,7位烯丙位氧化合成了目标化合物3,3,17,17-亚乙二氧基-7-羰基-雄烯二酮,总收率为45.2%。目标化合物和中间体的结构经IR,1 H NMR和MS确证。3,3,17,17-亚乙二氧基-7-羰基-雄烯二酮烯丙位氧化的最佳合成条件如下:n(PDC)∶n(t-BuOOH)∶n(3,3,17,17-亚乙二氧基-雄烯二酮)=4∶4∶1,反应温度为25℃,反应时间为5h。此合成方法反应原料易得,反应条件温和且产率高。
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| 关 键 词： | 雄烯二酮 烯丙位氧化 重铬酸的吡啶盐 |
Synthesis of 3,3,17,17-bis(ethylenedioxy)-androsten-7-one |
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| CHEN Shao-rui.Synthesis of 3,3,17,17-bis(ethylenedioxy)-androsten-7-one[J].Hebei Journal of Industrial Science & Technology,2012,29(6):370-372,375. |
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| Authors: | CHEN Shao-rui |
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| Institution: | CHEN Shao-rui(College of Sciences,Hebei University of Science and Technology,Shijiazhuang Hebei 050018,China) |
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| Abstract: | The title compound 3,3,17,17-bis(ethylenedioxy)-androsten-7-one was synthesized from androstenedione by acetalization of 3,17-carbonyl groups and oxydation of 7-methylene.The target product and intermediates were identified by IR,1H NMR and MS.The total yield of the title compound was 45.2%,which was obtained under optimized conditions: n(PDC)∶n(t-BuOOH)∶n(3,3,17,17-bis(ethylenedioxy)-androstenedi-one)=4∶4∶1,reaction temperature of 25 ℃ and reaction time of 5 h.This method has such advantages of mild condition,simple operation and high yield. |
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| Keywords: | androstenedione allylic oxidation PDC |
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