Mechanochemically Induced Conversion of Crystalline Benzamide Polymorphs by Seeding

Mechanochemically Induced Conversion of Crystalline Benzamide Polymorphs by Seeding
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DOI:
10.1002/anie.201607358
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发表时间:
2016-11-07
影响因子:
16.6
通讯作者:
Emmerling, Franziska
Emmerling, Franziska
中科院分区:
化学1区
文献类型:
--
作者:
Fischer, Franziska;Greiser, Sebastian;Emmerling, Franziska

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苯甲酰胺因其多晶型而闻名近200年。描述了三种多晶型物。迄今为止,仅可能在混合物中结晶亚稳态形式与结晶学上最稳定的形式I。通过机械化学处理实现了I型完全转化为亚稳态III型。催化量的烟酰胺晶种用于通过机械化学晶种活化转化。NMR实验表明,在转化过程中,烟酰胺分子以统计学方式掺入苯甲酰胺III型的晶格中。使用原位粉末X射线衍射的转化途径进行了评价。
Benzamide has been known for its polymorphism for almost 200 years. Three polymorphic forms are described. To date, it was only possible to crystallize a metastable form in a mixture together with the thermodynamically most stable form I. A complete transformation of form I into the metastable form III by mechanochemical treatment has been achieved. Catalytic amounts of nicotinamide seeds were used to activate the conversion by mechanochemical seeding. NMR experiments indicated that the nicotinamide molecules were incorporated statistically in the crystal lattice of benzamide form III during the conversion. The transformation pathway was evaluated using in situ powder X-ray diffraction.