| C-(6,11-二氢-5H-二苯[b,e]氮杂卓-6-烷)-甲胺的合成研究 |
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| 引用本文： | 李国庆,胡艳芳,马晓梅,聂兆广,邢雅成.C-(6,11-二氢-5H-二苯[b,e]氮杂卓-6-烷)-甲胺的合成研究[J].青岛大学学报(自然科学版),2007,20(1):47-51. |
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| 作者姓名： | 李国庆 胡艳芳 马晓梅 聂兆广 邢雅成 |
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| 作者单位： | 青岛大学化学化工与环境学院,青岛,266071 |
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| 摘 要： | C-（6，11-二氢-5H-二苯b，e]氮杂卓-6-烷）-甲胺是盐酸依匹斯汀的重要中间体，它是由5，11-二苯b，e]氮杂卓-6-腈经过还原反应制得，是合成该药的关键步骤。为此考察了氢化锂铝和红铝两种还原剂的还原效果，还考察了底物与还原剂的摩尔比，反应温度，反应时间等工艺条件。结果发现氢化锂铝的还原效果比较理想，并确定了较佳的工艺参数：当底物与还原剂的摩尔比为1：4，反应温度为20℃，反应时间为2h，产物的质量百分比收率可达92．7％。并通过IR，^1H—NMR对目标产物进行了表征。该反应对反应条件要求比较苛刻，比较适合实验室操作及小规模生产。
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| 关 键 词： | 依匹斯汀 中间体 还原反应 氢化锂铝 |
| 文章编号： | 1006-1037（2007）01-0047-05 |
| 收稿时间： | 2006-10-21 |
| 修稿时间： | 2006-10-21 |
Synthesis of C-(6,11-Dihydro-5H-dibenzo[b,e]azepin-6-yl)-methylamine |
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| LI Guo-qing,HU Yan-fang,MA Xiao-mei,NIE Zhao-guang,XING Ya-cheng.Synthesis of C-(6,11-Dihydro-5H-dibenzo[b,e]azepin-6-yl)-methylamine[J].Journal of Qingdao University(Natural Science Edition),2007,20(1):47-51. |
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| Authors: | LI Guo-qing HU Yan-fang MA Xiao-mei NIE Zhao-guang XING Ya-cheng |
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| Institution: | College of Chemical Engineering and Environmental Science, Qingdao University, Qingdao 266071, China |
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| Abstract: | C-(6,11-Dihydro-5H-dibenzob,e]azepin-6-yl)-methylamine was an important intermediate product of Epinastine hydrochloride.It was obtained with 5,11-Dibenzoazepine-6-carbonitrile as primary material through reduction.During the whole reducing process two reducing agents(LiAlH4 and SDMA) were contrasted to determine which was better,and LiAlH4(lithium aluminohydride)was chosen for its better reductivity and higher yield.The dosage of reducing agent and the reducing temperature and time were also been validated for better technological parameters.The structure of the final product was proved by IR and 1H-NMR. |
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| Keywords: | epinastine hydrochloride intermediate product reduction lithium aluminohydride |
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