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化学工业与工程 2018, Vol. 35 Issue (3) :38-42    DOI: 10.13353/j.issn.1004.9533.20182002
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依鲁替尼4种晶型的制备、表征与稳定性研究
徐悦1,2, 吴书平1, 陈真真1, 翟晶焕1, 陆杰1
1. 上海工程技术大学化学化工学院, 上海 201620;
2. 蔚山大学化工学院, 蔚山 44610, 韩国
Preparation, Characterization and Stability of Four Solid Forms of Ibrutinib
Xu Yue1,2, Wu Shuping1, Chen Zhenzhen1, Zhai Jinghuan1, Lu Jie1
1. School of Chemistry and Chemical Engineering, Shanghai University of Engineering Science, Shanghai 201620, China;
2. School of Chemical Engineering, University of Ulsan, Ulsan 44610, Korea

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摘要 

制备了依鲁替尼的4种晶型(晶型A、晶型B、晶型C和假多晶型苯甲醚溶剂化物),采用粉末X-射线衍射分析、红外光谱分析、热分析技术对依鲁替尼4种晶型进行了固相表征,并通过混悬实验筛选出稳定晶型。结果表明,依鲁替尼4种晶型的理化性质存在明显差异,无溶剂晶型间的稳定性关系为:晶型A > 晶型C > 晶型B,晶型A为热力学稳定晶型。

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徐悦
吴书平
陈真真
翟晶焕
陆杰
关键词依鲁替尼;   多晶型;   表征;   稳定性     
Abstract

In this work, four solid forms of ibrutinib (form A, form B, form C and pseudo-polymorph anisole solvate) were prepared. The solid forms were characterized by X-ray diffraction, infrared spectroscopy and thermal analysis, and the stable form was selected by suspension experiments. The results show that the chemical and physical properties of the four forms of ibrutinib have obvious differences. The stability relationship of anhydrous forms is:form A>form C>form B, and form A is the thermodynamic stable crystalline form.

Keywordsibrutinib;   polymorph;   characterization;   stability     
Received 2017-12-20;
Fund:

国家自然科学基金(21476136)、上海市科委重点支撑项目(15430501200)以及中德科学基金(GZ935)。

Corresponding Authors: 陆杰,E-mail:dr.lujie@foxmail.com。     Email: dr.lujie@foxmail.com
About author: 徐悦(1993-),女,博士研究生。
引用本文:   
徐悦, 吴书平, 陈真真, 翟晶焕, 陆杰.依鲁替尼4种晶型的制备、表征与稳定性研究[J].  化学工业与工程, 2018,35(3): 38-42
Xu Yue, Wu Shuping, Chen Zhenzhen, Zhai Jinghuan, Lu Jie.Preparation, Characterization and Stability of Four Solid Forms of Ibrutinib[J].  Chemcial Industry and Engineering, 2018,35(3): 38-42
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