| 药物中间体二硫化二苯并噻唑的合成 |
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| 引用本文： | 杨兰,陈学玺,朱永健. 药物中间体二硫化二苯并噻唑的合成[J]. 青岛科技大学学报(自然科学版), 2007, 28(4): 283-286,293 |
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| 作者姓名： | 杨兰 陈学玺 朱永健 |
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| 作者单位： | 青岛科技大学,化工学院,山东,青岛,266042;青岛科技大学,化工学院,山东,青岛,266042;青岛科技大学,化工学院,山东,青岛,266042 |
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| 摘 要： | 为制得高品质医药中间体二硫化二苯并噻唑(DM),采用环境友好型氧化剂H2O2和有机溶剂,将二巯基苯并噻唑(M)一步氧化得到DM。通过对反应时间、反应温度、物料配比等因素进行考察,最终得到最佳工艺条件:温度40℃,加料时间1 h,反应时间3 h,碳酸钠5%(以M重量为基准),n(M)∶n(H2O2)=2∶1.1,有机溶剂3倍(以M重量为基准)。在此条件下,DM的熔点可达185℃,纯度高达99%,加入极少量表面活性剂,使最终产率高达96%。
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| 关 键 词： | 过氧化氢 氧化 二硫化二苯并噻唑 |
| 文章编号： | 1672-6987（2007）-04-0283-04 |
| 收稿时间： | 2006-12-28 |
| 修稿时间： | 2006-12-28 |
Synthesis of Medical Intermediate Dibenzothiazole Disulfide |
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| YANG Lan,CHEN Xue-xi,ZHU Yong-jian. Synthesis of Medical Intermediate Dibenzothiazole Disulfide[J]. Journal of Qingdao University of Science and Technology:Natutral Science Edition, 2007, 28(4): 283-286,293 |
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| Authors: | YANG Lan CHEN Xue-xi ZHU Yong-jian |
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| Affiliation: | College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China |
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| Abstract: | Dibenzothiazole disulfide(DM) was prepared using dimercaptobenzothiazole(M) as starting material,H2O2 as oxidizing agent and an organic compound as solvent by one-step method.The effects of factors such as reaction time,temperature and the ratio of reactants etc.on reaction results were studied.The obtained optimum reaction conditions were reaction temperature 40℃,dosage of sodium carbonate 5%(based on M),the ratio of M to H2O2 2∶1.1,the ratio of solvent to M 3∶1,addition time 1 h,reaction time 3 h.Under above conditions,the yields was 96% and the purity and melting point of obtained product were 99% and 185℃ respectively. |
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| Keywords: | hydrogen peroxide oxidation dibenzothiazole disulfide |
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