| 5a-雄甾-2-烯-17-酮的合成 |
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| 引用本文： | 左前进,吴来喜,申利群.5a-雄甾-2-烯-17-酮的合成[J].工业催化,2010,18(12):55-57. |
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| 作者姓名： | 左前进 吴来喜 申利群 |
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| 作者单位： | 1.邵阳科瑞化学品有限公司,湖南 邵阳 420000;2.广西民族大学化学与生态工程学院, 广西 南宁530006 |
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| 基金项目： | 广西自然科学基金，广西高校优秀人才资助项目 |
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| 摘 要： | 以表雄酮为原料,经苯磺酰氯磺酰化,在二甲基甲酰胺溶剂中用4-二甲氨基吡啶作为催化剂消除苯磺酸,合成了5a-雄甾-2-烯-17-酮,考察反应温度、反应时间、溶剂和催化剂用量等因素对反应的影响。结果表明,表雄酮苯磺酸酯的合成最佳反应时间为30 h,脱苯磺酸合成5a-雄甾-2-烯-17-酮的最佳反应条件为:反应温度70℃,反应时间60 min,溶剂用量7.5 mL,催化剂4-二甲氨基吡啶用量0.3 g。在此条件下,5a-雄甾-2-烯-17-酮总收率达92.0%。
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| 关 键 词： | 催化化学 表雄酮 5a-雄甾-2-烯-17-酮合成 4-二甲氨基吡啶
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Synthesis of 5a-androst-2-en-17-one |
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| ZUO Qianjin,WU Laixi,SHEN Liqun.Synthesis of 5a-androst-2-en-17-one[J].Industrial Catalysis,2010,18(12):55-57. |
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| Authors: | ZUO Qianjin WU Laixi SHEN Liqun |
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| Affiliation: | 1.Shaoyang Kerey Chemicals Co.,Ltd.,Shaoyang 420000, Hunan, China; 2.College of Chemistry and ;Ecological Engineering, Guangxi University for Nationalities, Nanning 530006, Guangxi, China |
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| Abstract: | 5a-Androst-2-en-17-one was synthesized via the sulfonylation of 5a-androsterone and then elimination of benzene sulfonic acid with 4-dimethylaminopyridine as the catalyst. The influence of reaction temperature, reaction time, the dosage of the solvent and the catalyst was investigated. The results showed that the optimal time for the sulfonylation of 5a-androsterone was 30 h; the total yield of 5a-andro- st-2-en-17-one reached 92.2% under the optimum reaction condition of elimination of benzene sulfonic acid to synthesize 5a-androst-2-en-17-one as follows：reaction temperature 70 ℃, reaction time 60 min, solvent amount 7.5 mL, and 4-dimethylaminopyridine dosage 0.3 g. |
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| Keywords: | catalytic chemistry epiandrosterone 5a-androst-2-en-17-one synthesis 4-dimethylaminopyridine |
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