| 四氢萘类化合物合成工艺研究 |
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| 引用本文： | 付丙月,唐辉,郑灿辉,刘嘉,周峰,周有骏,朱驹,吕加国.四氢萘类化合物合成工艺研究[J].药学实践杂志,2012,30(1):35-37. |
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| 作者姓名： | 付丙月 唐辉 郑灿辉 刘嘉 周峰 周有骏 朱驹 吕加国 |
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| 作者单位： | 1. 第二军医大学药学院药物化学教研室,上海,200433
2. 山东大学附属省立医院,山东济南,250021 |
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| 基金项目： | 国家自然科学基金(20972187). |
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| 摘 要： | 目的 优化取代四氢萘类化合物的合成工艺,重点考察10%Pd/C对关键中间体合成的影响。 方法 平行试验比较10%Pd/C和三乙基硅烷催化羰基还原反应,并对实验结果进行总体分析;对10%Pd/C催化还原采用正交设计法,考察反应物与10%Pd/C的投料比例及溶剂对收率的影响。 结果 10%Pd/C催化羰基还原的成本明显低于三乙基硅烷,且收率高,杂质少,易处理;正交试验证实,催化剂与反应物的投料比例对反应的影响最为显著。 结论 实验证实,利用10%Pd/C催化还原关键中间体,使得取代四氢萘类化合物的合成路线更加
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| 关 键 词： | 取代四氢萘 合成 正交设计 |
| 收稿时间： | 2011/1/20 0:00:00 |
| 修稿时间： | 2011/9/29 0:00:00 |
Synthesis of substituted tetrahydronaphthalene |
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| FU Bing-yue,TANG Hui,ZHENG Can-hui,LIU Ji,ZHOU Feng,ZHOU You-jun,ZHU Ju and LV Jia-guo.Synthesis of substituted tetrahydronaphthalene[J].The Journal of Pharmaceutical Practice,2012,30(1):35-37. |
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| Authors: | FU Bing-yue TANG Hui ZHENG Can-hui LIU Ji ZHOU Feng ZHOU You-jun ZHU Ju and LV Jia-guo |
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| Institution: | Department of Medicinal Chemistry, School of Pharmacy, Second Military Medical University, Shanghai 200433, China;Provincial Hospital Affiliated to Shandong University, Jinan 250021, China;Department of Medicinal Chemistry, School of Pharmacy, Second Military Medical University, Shanghai 200433, China;Department of Medicinal Chemistry, School of Pharmacy, Second Military Medical University, Shanghai 200433, China;Department of Medicinal Chemistry, School of Pharmacy, Second Military Medical University, Shanghai 200433, China;Department of Medicinal Chemistry, School of Pharmacy, Second Military Medical University, Shanghai 200433, China;Department of Medicinal Chemistry, School of Pharmacy, Second Military Medical University, Shanghai 200433, China;Department of Medicinal Chemistry, School of Pharmacy, Second Military Medical University, Shanghai 200433, China |
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| Abstract: | Objective To optimize the synthesis of substituted tetrahydronaphthalene and investigate the influence of 10% Pd/C catalyst in the synthesis of key intermediate. Methods A parallel test was carried out to compare the catalytic activity of triethyl silicane and the 10% Pd/C catalyst, including the total analysis of experimental result . And orthogonal experimental design was used and the influence of solvent and reactant ratio on the yield were investigated. Results The cost of the 10% Pd/C catalyst was obviously lower than that of triethyl silicane,with high yield, little impurity easy effluent disposal. Orthogonal test confirms that the ratio of reactant and catalystthe was the most significant factor. Conclusion The experiments proved that the optimal preparation procedure was much more available for industrial production using the 10% Pd/C as a catalyst. |
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| Keywords: | substituted tetrahydronaphthalene synthesis orthogonal design |
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