A comprehensive study on the efficient one-pot synthesis of polyhedral octaphenylsilsesquioxane (OPS) is reported via the hydrolytic condensation of phenyltrimethoxysilane (PTMS) in the presence of basic catalyst to i...A comprehensive study on the efficient one-pot synthesis of polyhedral octaphenylsilsesquioxane (OPS) is reported via the hydrolytic condensation of phenyltrimethoxysilane (PTMS) in the presence of basic catalyst to investigate the specific synthesis mechanism.The synthetic reactions are monitored with real time infrared (RTIR) spectroscopy.Then RTIR coupled with 29Si nuclear magnetic resonance spectroscopy (NMR) and matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF-MS) are used to monitor the reactions and identify the intermediary species during the reaction.The rapid hydrolysis of PTMS is detected by RTIR.Contrary to previous reports,the ladder-like structured species are identified as intermediates during the reaction process.it is suggested that formation of caged T8OPS is realized through the chain break and rearrangement of the ladder-like phenyltrimethoxysilanes.Accordingly,a scheme from hydrolysis of the PTMS to formation of the OPS is provided.展开更多
基金This work was funded by grants from the China Postdoctoral Science Foundation funded project(Grant No.2018M631353)National Science Foundation for Young Scholars of China(Grant No.51803008).
文摘A comprehensive study on the efficient one-pot synthesis of polyhedral octaphenylsilsesquioxane (OPS) is reported via the hydrolytic condensation of phenyltrimethoxysilane (PTMS) in the presence of basic catalyst to investigate the specific synthesis mechanism.The synthetic reactions are monitored with real time infrared (RTIR) spectroscopy.Then RTIR coupled with 29Si nuclear magnetic resonance spectroscopy (NMR) and matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF-MS) are used to monitor the reactions and identify the intermediary species during the reaction.The rapid hydrolysis of PTMS is detected by RTIR.Contrary to previous reports,the ladder-like structured species are identified as intermediates during the reaction process.it is suggested that formation of caged T8OPS is realized through the chain break and rearrangement of the ladder-like phenyltrimethoxysilanes.Accordingly,a scheme from hydrolysis of the PTMS to formation of the OPS is provided.
