| 阿替美唑盐酸盐合成工艺的改进 |
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| 引用本文： | 李斌,薛峰,居沈贵. 阿替美唑盐酸盐合成工艺的改进[J]. 精细化工, 2016, 33(3) |
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| 作者姓名： | 李斌 薛峰 居沈贵 |
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| 作者单位： | 南京工业大学化工学院,南京工业大学化工学院,南京工业大学 化工学院 |
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| 基金项目： | 国家自然科学基金（批准号：21176118） |
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| 摘 要： | 以2-(2-溴乙酰基)-2-乙基茚酮为原料经过咪唑成环,羰基还原,最后盐酸化合成盐酸阿替美唑,总收率58%。其各步中间体结构经1HNMR、MS分析测试技术确证。改进了咪唑成环过程工艺条件,并考察了反应温度对收率的影响,确定了最佳反应条件:反应温度140℃,通氨气,反应时间4 h,将咪唑成环反应的收率由50%提高至72%。对于羰基还原过程采用黄鸣龙还原法替代原有的钯碳还原法,采用正交实验法优化了反应条件,确定了最优的工艺条件:反应溶剂为二甘醇,反应温度190℃,n(氢氧化钾)∶n〔4-(2-乙基-2-茚酮)咪唑〕=2∶1,n(水合肼)∶n〔4-(2-乙基-2-茚酮咪唑〕=7∶1,收率为81%。
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| 关 键 词： | 咪唑成环 黄鸣龙还原法 盐酸阿替美唑 正交实验法 医药原料 |
| 收稿时间： | 2015-12-17 |
| 修稿时间： | 2016-01-18 |
Improved Synthesis of Atipamzole Hydrochloride |
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| LI Bin,XUE Feng and JU Shen Gui. Improved Synthesis of Atipamzole Hydrochloride[J]. Fine Chemicals, 2016, 33(3) |
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| Authors: | LI Bin XUE Feng JU Shen Gui |
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| Affiliation: | chool of chemical engineering, Nanjing University of Technology,School of chemical engineering, Nanjing University of Technology,School of chemical engineering, Nanjing University of Technology |
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| Abstract: | Atipamzole Hydrochloride was synthesized from 2 - (2 - bromine acetyl) - 2 - ethylindanone through three-step reations includingthe imidazole ring formation, carbonyl reduction and hydrochloric acid .The technological conditions of imidazole ring formation were improved, and the effect of reaction temperature on the yield was investigated, Determined the optimum reaction conditions .The yield of the reaction was increased to 72%. In the process of reduction of the carbonyl group, the method of Huang Minglong reduction was used to replace the original palladium carbon reduction method, and the reaction conditions were optimized by orthogonal experiment. The optimum technological conditions were determined |
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| Keywords: | Huang Minglong reduction method imidazole ring formation Atipamzole hydrochloride Orthogonal experimental method |
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