Investigation of ethylene oxide oligomerization during functionalization of poly(styryl)lithium using MALDI-TOF MS and NMR

Roderic P. Quirk; Robert T. Mathers; Chrys Wesdemiotis; Mark A. Arnould

doi:10.1021/ma011978z

Investigation of ethylene oxide oligomerization during functionalization of poly(styryl)lithium using MALDI-TOF MS and NMR

Roderic P. Quirk, Robert T. Mathers, Chrys Wesdemiotis, Mark A. Arnould

Penn State New Kensington

Research output: Contribution to journal › Article › peer-review

56 Scopus citations

Abstract

The amount of ethylene oxide oligomerization for functionalization of poly(styryl)lithium in benzene at 25 °C has been determined using MALDI-TOF MS and ¹H and ¹³C NMR. Chemically insignificant amounts of oligomer were found using 4 equiv of ethylene oxide ([EO]/[PLi]) after 12 h. For reactions times ranging from 12 h to 4 weeks using 10 equiv of ethylene oxide, the corresponding amounts of dimeric oligomerization varied from 4% to 34%. Trimeric oligomerization of ethylene oxide was detected after 1 week (1%) and 4 weeks (4%) by MALDI-TOF MS. The quantitative results from MALDI-TOF MS were in good agreement with results from both ¹H and ¹³C NMR analyses. The quantitative aspects of MALDI-TOF MS compared to ¹H and ¹³C NMR for the determination of the amount of EO oligomerization have been established through the synthesis and characterization of the model dimeric oligomer product, ω-(2-(2-hydroxyethoxy)ethyl)polystyrene.

Original language	English (US)
Pages (from-to)	2912-2918
Number of pages	7
Journal	Macromolecules
Volume	35
Issue number	8
DOIs	https://doi.org/10.1021/ma011978z
State	Published - Apr 9 2002

All Science Journal Classification (ASJC) codes

Organic Chemistry
Polymers and Plastics
Inorganic Chemistry
Materials Chemistry

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@article{81ec399d6024470eb2cc6bcbc72fc9b5,

title = "Investigation of ethylene oxide oligomerization during functionalization of poly(styryl)lithium using MALDI-TOF MS and NMR",

abstract = "The amount of ethylene oxide oligomerization for functionalization of poly(styryl)lithium in benzene at 25 °C has been determined using MALDI-TOF MS and 1H and 13C NMR. Chemically insignificant amounts of oligomer were found using 4 equiv of ethylene oxide ([EO]/[PLi]) after 12 h. For reactions times ranging from 12 h to 4 weeks using 10 equiv of ethylene oxide, the corresponding amounts of dimeric oligomerization varied from 4% to 34%. Trimeric oligomerization of ethylene oxide was detected after 1 week (1%) and 4 weeks (4%) by MALDI-TOF MS. The quantitative results from MALDI-TOF MS were in good agreement with results from both 1H and 13C NMR analyses. The quantitative aspects of MALDI-TOF MS compared to 1H and 13C NMR for the determination of the amount of EO oligomerization have been established through the synthesis and characterization of the model dimeric oligomer product, ω-(2-(2-hydroxyethoxy)ethyl)polystyrene.",

author = "Quirk, {Roderic P.} and Mathers, {Robert T.} and Chrys Wesdemiotis and Arnould, {Mark A.}",

year = "2002",

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T1 - Investigation of ethylene oxide oligomerization during functionalization of poly(styryl)lithium using MALDI-TOF MS and NMR

AU - Quirk, Roderic P.

AU - Mathers, Robert T.

AU - Wesdemiotis, Chrys

AU - Arnould, Mark A.

PY - 2002/4/9

Y1 - 2002/4/9

N2 - The amount of ethylene oxide oligomerization for functionalization of poly(styryl)lithium in benzene at 25 °C has been determined using MALDI-TOF MS and 1H and 13C NMR. Chemically insignificant amounts of oligomer were found using 4 equiv of ethylene oxide ([EO]/[PLi]) after 12 h. For reactions times ranging from 12 h to 4 weeks using 10 equiv of ethylene oxide, the corresponding amounts of dimeric oligomerization varied from 4% to 34%. Trimeric oligomerization of ethylene oxide was detected after 1 week (1%) and 4 weeks (4%) by MALDI-TOF MS. The quantitative results from MALDI-TOF MS were in good agreement with results from both 1H and 13C NMR analyses. The quantitative aspects of MALDI-TOF MS compared to 1H and 13C NMR for the determination of the amount of EO oligomerization have been established through the synthesis and characterization of the model dimeric oligomer product, ω-(2-(2-hydroxyethoxy)ethyl)polystyrene.

AB - The amount of ethylene oxide oligomerization for functionalization of poly(styryl)lithium in benzene at 25 °C has been determined using MALDI-TOF MS and 1H and 13C NMR. Chemically insignificant amounts of oligomer were found using 4 equiv of ethylene oxide ([EO]/[PLi]) after 12 h. For reactions times ranging from 12 h to 4 weeks using 10 equiv of ethylene oxide, the corresponding amounts of dimeric oligomerization varied from 4% to 34%. Trimeric oligomerization of ethylene oxide was detected after 1 week (1%) and 4 weeks (4%) by MALDI-TOF MS. The quantitative results from MALDI-TOF MS were in good agreement with results from both 1H and 13C NMR analyses. The quantitative aspects of MALDI-TOF MS compared to 1H and 13C NMR for the determination of the amount of EO oligomerization have been established through the synthesis and characterization of the model dimeric oligomer product, ω-(2-(2-hydroxyethoxy)ethyl)polystyrene.

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U2 - 10.1021/ma011978z

DO - 10.1021/ma011978z

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JO - Macromolecules

JF - Macromolecules

IS - 8

ER -

Investigation of ethylene oxide oligomerization during functionalization of poly(styryl)lithium using MALDI-TOF MS and NMR

Abstract

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