NMR characterisation of structure in solvates and polymorphs of formoterol fumarate.
NMR characterisation of structure in solvates and polymorphs of formoterol fumarate.
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富马酸福莫特罗溶剂化物和多晶型物结构的 NMR 表征。
DOI：
10.1002/mrc.3862
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发表时间：
2012
期刊：
影响因子：
--
通讯作者：
Apperley DC
中科院分区：
文献类型：
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作者：
Apperley DC
采用核磁共振技术对富马酸福莫特罗的两种多晶型和两种醇（乙醇和异丙醇）的固态结构进行了研究。第一性原理屏蔽计算与核磁共振数据相结合，成功地将峰与溶剂化物的晶体位置联系起来，包括处于等效分子位置的原子。在不对称单元中发现了一种非特征性结构的asolate形式C含有一个formoterol离子和半个富马酸盐离子。乙醇酸盐和形式C的HETCOR实验可以确定质子的化学位移，并提高了前一种化合物的13c分辨率。在核磁共振实验条件下，监测了溶剂化物脱溶生成C的过程。在不同的形式下观察到苯基环翻转的不同速率。碳- 13弛豫时间和2h核磁共振用于探测富马酸盐离子的动力学。版权所有©2012 John Wiley & Sons， Ltd。
The solid‐state structures of two polymorphs and two alcoholates (ethanol and isopropanol) of formoterol fumarate have been investigated by a combination of NMR techniques. First‐principles shielding computations are combined with NMR data to successfully relate peaks to their crystallographic positions for the solvates, including atoms that are in equivalent molecular positions. The uncharacterised structure of the asolvate form C is found to contain a single formoterol ion and half a fumarate ion in its asymmetric unit. HETCOR experiments for the ethanolate and form C allow proton chemical shifts to be determined and give improved13C resolution for the former compound. Desolvation of the solvates to form C has been monitored under the conditions of the NMR experiment. Differential rates of phenylene ring flipping are observed in the different forms. Carbon‐13 relaxation times and2H NMR are used to probe dynamics of the fumarate ion. Copyright © 2012 John Wiley & Sons, Ltd.