One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products

The NaOH-catalyzed hydrolytic condensation of the reaction product between N-(βaminoethyl)-γ-aminopropyltrimethoxysilane and phenyl glycidyl ether (PGE) was followed by matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry (UV-MALDI-TOF MS) and electrospray ionizat...

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Detalles Bibliográficos
Autor principal: Erra Balsells, Rosa
Publicado: 2001
Materias:
Electrospray ionization
Laser desorption
Condensation
Dehydration
Desorption
Ethers
Hydrolysis
Mass spectrometry
Synthesis (chemical)
Ultraviolet radiation
Silanes
Acceso en línea:https://bibliotecadigital.exactas.uba.ar/collection/paper/document/paper_00249297_v34_n11_p3534_Fasce
http://hdl.handle.net/20.500.12110/paper_00249297_v34_n11_p3534_Fasce
Aporte de:
Biblioteca Digital - Facultad de Ciencias Exactas y Naturales (UBA) de Universidad de Buenos Aires
id paper:paper_00249297_v34_n11_p3534_Fasce
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spelling paper:paper_00249297_v34_n11_p3534_Fasce2023-06-08T14:52:33Z One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products Erra Balsells, Rosa Electrospray ionization Laser desorption Condensation Dehydration Desorption Ethers Hydrolysis Mass spectrometry Synthesis (chemical) Ultraviolet radiation Silanes The NaOH-catalyzed hydrolytic condensation of the reaction product between N-(βaminoethyl)-γ-aminopropyltrimethoxysilane and phenyl glycidyl ether (PGE) was followed by matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry (UV-MALDI-TOF MS) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF MS). After 24 h at 50 °C, main condensation products were a mixture of perfect and imperfect polyhedra: T8, T9(OH), and T10, with traces of T7(OH) and T11(OH). Every one of these products was composed of a series of peaks in the mass spectra, accounting for the incomplete reaction of PGE with the aminosilane (e.g., T8 showed the presence of the species containing 24 PGE units arising from the complete reaction of the initial silane, as well as species containing 23, 22, and 21 PGE units). A thermal treatment to 150 °C led to the appearance of extra peaks corresponding to intramolecular dehydration products. Peaks corresponding to the loss of one water molecule from T9(OH) and T7(OH) were present and could be ascribed to the reaction between SiOH and a secondary OH group. Dehydration products from T8 and T10 were observed, as well as species arising from the loss of two water molecules from T9(OH) and T7(OH). A plausible explanation for the presence of these peaks is the rupture of a Si-O-Si bond in the presence of NaOH, followed by condensation of the resulting fragments with secondary OH groups. Fil:Erra-Balsells, R. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales; Argentina. 2001 https://bibliotecadigital.exactas.uba.ar/collection/paper/document/paper_00249297_v34_n11_p3534_Fasce http://hdl.handle.net/20.500.12110/paper_00249297_v34_n11_p3534_Fasce
institution Universidad de Buenos Aires
institution_str I-28
repository_str R-134
collection Biblioteca Digital - Facultad de Ciencias Exactas y Naturales (UBA)
topic Electrospray ionization
Laser desorption
Condensation
Dehydration
Desorption
Ethers
Hydrolysis
Mass spectrometry
Synthesis (chemical)
Ultraviolet radiation
Silanes
spellingShingle Electrospray ionization
Laser desorption
Condensation
Dehydration
Desorption
Ethers
Hydrolysis
Mass spectrometry
Synthesis (chemical)
Ultraviolet radiation
Silanes
Erra Balsells, Rosa
One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
topic_facet Electrospray ionization
Laser desorption
Condensation
Dehydration
Desorption
Ethers
Hydrolysis
Mass spectrometry
Synthesis (chemical)
Ultraviolet radiation
Silanes
description The NaOH-catalyzed hydrolytic condensation of the reaction product between N-(βaminoethyl)-γ-aminopropyltrimethoxysilane and phenyl glycidyl ether (PGE) was followed by matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry (UV-MALDI-TOF MS) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF MS). After 24 h at 50 °C, main condensation products were a mixture of perfect and imperfect polyhedra: T8, T9(OH), and T10, with traces of T7(OH) and T11(OH). Every one of these products was composed of a series of peaks in the mass spectra, accounting for the incomplete reaction of PGE with the aminosilane (e.g., T8 showed the presence of the species containing 24 PGE units arising from the complete reaction of the initial silane, as well as species containing 23, 22, and 21 PGE units). A thermal treatment to 150 °C led to the appearance of extra peaks corresponding to intramolecular dehydration products. Peaks corresponding to the loss of one water molecule from T9(OH) and T7(OH) were present and could be ascribed to the reaction between SiOH and a secondary OH group. Dehydration products from T8 and T10 were observed, as well as species arising from the loss of two water molecules from T9(OH) and T7(OH). A plausible explanation for the presence of these peaks is the rupture of a Si-O-Si bond in the presence of NaOH, followed by condensation of the resulting fragments with secondary OH groups.
author Erra Balsells, Rosa
author_facet Erra Balsells, Rosa
author_sort Erra Balsells, Rosa
title One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title_short One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title_full One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title_fullStr One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title_full_unstemmed One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title_sort one-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: uv-maldi-tof and esi-tof mass spectrometry characterization of reaction products
publishDate 2001
url https://bibliotecadigital.exactas.uba.ar/collection/paper/document/paper_00249297_v34_n11_p3534_Fasce
http://hdl.handle.net/20.500.12110/paper_00249297_v34_n11_p3534_Fasce
work_keys_str_mv AT errabalsellsrosa onestepsynthesisofpolyhedralsilsesquioxanesbearingbulkysubstituentsuvmalditofandesitofmassspectrometrycharacterizationofreactionproducts
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