| 依匹斯汀中间体6-氯-11H-二苯[b,e]氮杂卓的合成研究 |
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| 引用本文： | 李泉,李国庆,邢雅成. 依匹斯汀中间体6-氯-11H-二苯[b,e]氮杂卓的合成研究[J]. 应用化工, 2006, 35(9): 703-705 |
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| 作者姓名： | 李泉 李国庆 邢雅成 |
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| 作者单位： | 青岛大学,化学化工与环境学院,山东,青岛,266071 |
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| 摘 要： | 以5,11-二氢-二苯[b,e]氮杂卓-6-酮为原料,三氯氧磷为氯代试剂,以N,N-二甲基苯胺为缚酸剂,在无水的条件下,经过氯代反应合成6-氯-11H-二苯[b,e]氮杂卓,并通过IR1、H-NMR对6-氯-11H-二苯[b,e]氮杂卓进行了表征。研究了影响Ⅱ纯度及产率的因素。结果表明,适宜的合成条件为:5,11-二氢-二苯[b,e]氮杂卓-6-酮与三氯氧磷的摩尔比为1∶8,催化剂用量为0.6 mol的N,N-二甲基苯胺,控制反应温度130℃,反应5 h,用15%碳酸氢钠溶液,12%碳酸氢钠溶液和水各洗一次,可得到纯度理想、产率96%的6-氯-11H-二苯[b,e]氮杂卓。
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| 关 键 词： | 6-氯-11H-二苯[b,e]氮杂卓 三氯氧磷 氯代反应 无水 |
| 文章编号： | 1671-3206(2006)09-0703-03 |
| 收稿时间： | 2006-07-04 |
| 修稿时间： | 2006-07-04 |
Study of the synthesis methodology for intermediate product hydrochloride 6-chloro-11H-dibenzo[ b, e ] azepine of epinastine |
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| LI Quan,LI Guo-qing,XING Ya-cheng. Study of the synthesis methodology for intermediate product hydrochloride 6-chloro-11H-dibenzo[ b, e ] azepine of epinastine[J]. Applied chemical industry, 2006, 35(9): 703-705 |
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| Authors: | LI Quan LI Guo-qing XING Ya-cheng |
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| Affiliation: | College of Chemistry, Chemical Engineering and Environmental Science, Qingdao University, Qingdao 266071, China |
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| Abstract: | This thesis is about the synthesis methodology for the important intermediate product hydrochloride 6-chloro-11H-dibenzoazepine of epinastine.The intermediate product was obtained with 5,11-dihydro-dibenzoazepin-6-ketone as primary material through POCl_3 chlorination at N,N-dimethylaniline as activator and sine aq situation.Use IR,~1H NMR to analyze the product.The factors influencing the purity and yield of product 6-chloro-11H-dibenzoazepine were studied.The results showed that 5,11-dihydro-dibenzoazepin-6-ketone∶POCl_3∶N,N-dimethylaniline 1∶8∶0.6,reacting(5 h) at 130℃,quickly using 15%NaHCO_3,12% NaHCO_3 and water neutralizing to post processing could get desired purity and 96% yield of intermediate product 6-chloro-11H-dibenzoazepine. |
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| Keywords: | 6-chloro-11 H-dibenzo[b e]azepine phosphorus oxychloride chlorination anhydrous |
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