Hamad H Al Mamari, Shamsaa Al Sulaimi, Lina Mardiana, Paul G Waddell, Michael J Hall
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引用次数: 0
摘要
最近一篇关于 Ru 催化 4-氨基安替比林（AP）C-H 键芳基化反应的文章报道了 AP 苯甲酰胺的合成。为了给已发表的 AP 苯甲酰胺结构提供更多支持，我们采用了高通量（HTP）封装纳米液滴结晶（ENaCt）技术。这使得通过单晶 X 射线衍射分析（SCXRD）确定结构成为可能。本文介绍了 N-(1,5-二甲基-3-氧代-2-苯基-2,3-二氢-1H-吡唑-4-基)-2-甲基苯甲酰胺（C19H19N3O2）的结晶和 X 射线晶体结构，为含有 4-氨基安替比林的苯甲酰胺提供了结构确认。X 射线结构分析显示 AP 苯甲酰胺 N-H 质子与 AP 分子的羰基 O 原子之间存在分子间氢键相互作用。
High-throughput crystallization and crystal structure of N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-methylbenzamide: a benzamide bearing the 4-aminoantipyrine moiety.
A recent communication on Ru-catalyzed C-H bond arylation with 4-aminoantipyrine (AP) reported the synthesis of AP benzamides. In order to provide additional support to the published structures of AP benzamides, crystallization by high-throughput (HTP) encapsulated nanodroplet crystallization (ENaCt) was undertaken. This allowed for conclusive structure determination by single-crystal X-ray diffraction analysis (SCXRD). This article describes the crystallization and X-ray crystal structure of N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-methylbenzamide, C19H19N3O2, as a benzamide bearing 4-aminoantipyrine, providing structural confirmation. X-ray structure analysis reveals intermolecular hydrogen-bonding interactions between the AP benzamide N-H proton and the carbonyl O atom of the AP moiety.
期刊介绍：
Acta Crystallographica Section C: Structural Chemistry is continuing its transition to a journal that publishes exciting science with structural content, in particular, important results relating to the chemical sciences. Section C is the journal of choice for the rapid publication of articles that highlight interesting research facilitated by the determination, calculation or analysis of structures of any type, other than macromolecular structures. Articles that emphasize the science and the outcomes that were enabled by the study are particularly welcomed. Authors are encouraged to include mainstream science in their papers, thereby producing manuscripts that are substantial scientific well-rounded contributions that appeal to a broad community of readers and increase the profile of the authors.
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