We followed the reactivity of acetone with 3‐aminopropyltrimethoxysilane, a potential organosilane coupling agent, by 1H, 13C and 29Si NMR spectroscopy. Selective 1D and 2D‐edited NMR experiments significantly contributed to simplify the spectral complexity of reaction solution and elucidated molecular structures within progressive reaction phases. The course of the 3‐aminopropyltrimethoxysilane reaction with acetone was shown by a progressive decrease of both reactants, and a concomitant appearance of water and methanol, due to formation of imine and hydrolysis of alkoxysilane groups, respectively. The occurrence of multiple siloxane linkages in a progressively larger cross‐linked macromolecular structure was revealed by DOSY‐NMR experiments and new signals in 29Si‐NMR spectra at different reaction times. The NMR approach described here may be applied to investigate the reactivity of other γ‐aminopropylalkoxysilanes and contribute to define procedures for the preparation of silica‐based materials. Copyright © 2014 John Wiley & Sons, Ltd.

中文翻译：

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NMR 光谱显示丙酮诱导的 3-氨基丙基三甲氧基硅烷 (APTMS) 聚合

我们通过 1H、13C 和 29Si NMR 光谱跟踪了丙酮与 3-氨基丙基三甲氧基硅烷（一种潜在的有机硅烷偶联剂）的反应性。选择性 1D 和 2D 编辑 NMR 实验显着有助于简化反应溶液的光谱复杂性并阐明渐进反应阶段中的分子结构。3-氨基丙基三甲氧基硅烷与丙酮的反应过程表现为两种反应物的逐渐减少，并伴随着水和甲醇的出现，这分别是由于亚胺的形成和烷氧基硅烷基团的水解。通过 DOSY-NMR 实验和不同反应时间的 29Si-NMR 光谱中的新信号，揭示了在逐渐变大的交联大分子结构中存在多个硅氧烷键。这里描述的 NMR 方法可用于研究其他 γ-氨基丙基烷氧基硅烷的反应性，并有助于定义二氧化硅基材料的制备程序。版权所有 © 2014 John Wiley & Sons, Ltd.