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Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers

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Resumo:The synthesis of two 1,3‐bis(4‐ethynylbenzyloxy)calix[4]arenes, 5,11,17,23‐tetrakis(1,1‐dimethylethyl)‐25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene (1 ) and 25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene (2 ), was accomplished through Sonogashira coupling of appropriate calixarene derivatives. Methods for the polymerization of these bifunctional building blocks with Rh(I) as a catalyst, leading ultimately to conjugated polymers having calix[4]arene units incorporated into the main chain, were explored. Calixarenes 1 and 2 were efficiently polymerized with rhodium‐based initiators and afforded the conjugated polymers poly{5,11,17,23‐tetrakis(1,1‐dimethylethyl)‐25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene} (poly 1 ) and poly{25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene}. Depending on the conditions, high conversions and good yields were obtained. The effects of adding cocatalysts (NHEt2 and/or PPh3) were studied in connection with the number‐average molecular weight and the molecular weight distribution of the resultant polymer (poly 1 ) and tentatively correlated with the formation of low‐molecular‐weight materials. A catalytic system containing triphenylphosphine as the sole additive ([Rh(nbd)Cl]2; [Rh]/[PPh3] = 0.5) proved to be the best for the polymerization of p ‐tert ‐butylcalixarene compound 1 . Linear polymers having high number‐average molecular weights (up to 1.1 × 105 g mol−1) with low polydispersities were produced under these conditions. For debutylated homologue 2 , its polymerization was best carried out in the absence of any added cocatalyst. A cyclopolymerization route, comprising the intramolecular ring closing of the calix[4]arene pendant ethynyl groups followed by an intermolecular propagation step, is advanced to explain the results.
Autores principais:Costa, Alexandra I.
Outros Autores:Prata, José V.
Assunto:Calixarene Catalysis Conjugated polymers Cyclopolymerization Rhodium Sonogashira coupling
Ano:2006
País:Portugal
Tipo de documento:artigo
Tipo de acesso:acesso restrito
Instituição associada:Instituto Politécnico de Lisboa
Idioma:inglês
Origem:Repositório Científico do Instituto Politécnico de Lisboa
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author Costa, Alexandra I.
author2 Prata, José V.
author2_role author
author_facet Costa, Alexandra I.
Prata, José V.
author_role author
contributor_name_str_mv RCIPL
country_str PT
creators_json_txt [{\"Person.name\":\"Costa, Alexandra I.\",\"Person.identifier.orcid\":\"0000-0002-5518-6506\"},{\"Person.name\":\"Prata, José V.\",\"Person.identifier.orcid\":\"0000-0002-9068-2847\"}]
datacite.contributors.contributor.contributorName.fl_str_mv RCIPL
datacite.creators.creator.creatorName.fl_str_mv Costa, Alexandra I.
Prata, José V.
datacite.date.Accepted.fl_str_mv 2006-12-15T00:00:00Z
datacite.date.available.fl_str_mv 2020-06-09T15:59:51Z
datacite.date.embargoed.fl_str_mv 2020-06-09T15:59:51Z
datacite.rights.fl_str_mv http://purl.org/coar/access_right/c_16ec
datacite.subjects.subject.fl_str_mv Calixarene
Catalysis
Conjugated polymers
Cyclopolymerization
Rhodium
Sonogashira coupling
datacite.titles.title.fl_str_mv Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers
dc.contributor.none.fl_str_mv RCIPL
dc.creator.none.fl_str_mv Costa, Alexandra I.
Prata, José V.
dc.date.Accepted.fl_str_mv 2006-12-15T00:00:00Z
dc.date.available.fl_str_mv 2020-06-09T15:59:51Z
dc.date.embargoed.fl_str_mv 2020-06-09T15:59:51Z
dc.format.none.fl_str_mv application/pdf
dc.identifier.none.fl_str_mv http://hdl.handle.net/10400.21/11810
dc.language.none.fl_str_mv eng
dc.publisher.none.fl_str_mv Wiley
dc.rights.none.fl_str_mv http://purl.org/coar/access_right/c_16ec
dc.subject.none.fl_str_mv Calixarene
Catalysis
Conjugated polymers
Cyclopolymerization
Rhodium
Sonogashira coupling
dc.title.fl_str_mv Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers
dc.type.none.fl_str_mv http://purl.org/coar/resource_type/c_6501
description The synthesis of two 1,3‐bis(4‐ethynylbenzyloxy)calix[4]arenes, 5,11,17,23‐tetrakis(1,1‐dimethylethyl)‐25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene (1 ) and 25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene (2 ), was accomplished through Sonogashira coupling of appropriate calixarene derivatives. Methods for the polymerization of these bifunctional building blocks with Rh(I) as a catalyst, leading ultimately to conjugated polymers having calix[4]arene units incorporated into the main chain, were explored. Calixarenes 1 and 2 were efficiently polymerized with rhodium‐based initiators and afforded the conjugated polymers poly{5,11,17,23‐tetrakis(1,1‐dimethylethyl)‐25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene} (poly 1 ) and poly{25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene}. Depending on the conditions, high conversions and good yields were obtained. The effects of adding cocatalysts (NHEt2 and/or PPh3) were studied in connection with the number‐average molecular weight and the molecular weight distribution of the resultant polymer (poly 1 ) and tentatively correlated with the formation of low‐molecular‐weight materials. A catalytic system containing triphenylphosphine as the sole additive ([Rh(nbd)Cl]2; [Rh]/[PPh3] = 0.5) proved to be the best for the polymerization of p ‐tert ‐butylcalixarene compound 1 . Linear polymers having high number‐average molecular weights (up to 1.1 × 105 g mol−1) with low polydispersities were produced under these conditions. For debutylated homologue 2 , its polymerization was best carried out in the absence of any added cocatalyst. A cyclopolymerization route, comprising the intramolecular ring closing of the calix[4]arene pendant ethynyl groups followed by an intermolecular propagation step, is advanced to explain the results.
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organization_str_mv urn:organizationAcronym:ipl
person_str_mv Costa, Alexandra I.
Costa, Alexandra I.
https://www.ciencia-id.pt/4212-F7BF-D971
4212-F7BF-D971
http://orcid.org/0000-0002-5518-6506
0000-0002-5518-6506
Prata, José V.
Prata, José V.
https://www.ciencia-id.pt/C11A-9130-8981
C11A-9130-8981
http://orcid.org/0000-0002-9068-2847
0000-0002-9068-2847
publishDate 2006
publisher.none.fl_str_mv Wiley
reponame_str Repositório Científico do Instituto Politécnico de Lisboa
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spelling engWileypt_PTThe synthesis of two 1,3‐bis(4‐ethynylbenzyloxy)calix[4]arenes, 5,11,17,23‐tetrakis(1,1‐dimethylethyl)‐25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene (1 ) and 25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene (2 ), was accomplished through Sonogashira coupling of appropriate calixarene derivatives. Methods for the polymerization of these bifunctional building blocks with Rh(I) as a catalyst, leading ultimately to conjugated polymers having calix[4]arene units incorporated into the main chain, were explored. Calixarenes 1 and 2 were efficiently polymerized with rhodium‐based initiators and afforded the conjugated polymers poly{5,11,17,23‐tetrakis(1,1‐dimethylethyl)‐25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene} (poly 1 ) and poly{25,27‐bis(4‐ethynylbenzyloxy)‐26,28‐dihydroxycalix[4]arene}. Depending on the conditions, high conversions and good yields were obtained. The effects of adding cocatalysts (NHEt2 and/or PPh3) were studied in connection with the number‐average molecular weight and the molecular weight distribution of the resultant polymer (poly 1 ) and tentatively correlated with the formation of low‐molecular‐weight materials. A catalytic system containing triphenylphosphine as the sole additive ([Rh(nbd)Cl]2; [Rh]/[PPh3] = 0.5) proved to be the best for the polymerization of p ‐tert ‐butylcalixarene compound 1 . Linear polymers having high number‐average molecular weights (up to 1.1 × 105 g mol−1) with low polydispersities were produced under these conditions. For debutylated homologue 2 , its polymerization was best carried out in the absence of any added cocatalyst. A cyclopolymerization route, comprising the intramolecular ring closing of the calix[4]arene pendant ethynyl groups followed by an intermolecular propagation step, is advanced to explain the results.application/pdfpt_PTSynthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymersPersonalCosta, Alexandra I.DSpacehttp://dspace.org/items/5f3891cc-260d-41d3-b803-4fd17e3734bdDSpacehttp://dspace.org/items/5f3891cc-260d-41d3-b803-4fd17e3734bdCostaAlexandraCiência IDhttps://www.ciencia-id.pt4212-F7BF-D971ORCIDhttp://orcid.org0000-0002-5518-6506Scopus Author IDhttps://www.scopus.com8968446100PersonalPrata, José V.DSpacehttp://dspace.org/items/15e229f3-a619-4931-87eb-799091dc1601DSpacehttp://dspace.org/items/15e229f3-a619-4931-87eb-799091dc1601PrataJosé VirgílioCiência IDhttps://www.ciencia-id.ptC11A-9130-8981ORCIDhttp://orcid.org0000-0002-9068-2847Researcher IDhttps://www.researcherid.comB-7214-2008Scopus Author IDhttps://www.scopus.com9276778400HostingInstitutionOrganizationalRCIPLe-mailmailto:rcaap@sp.ipl.ptrcaap@sp.ipl.ptISSNIsPartOf0887-624XISSNIsPartOf1099-0518DOIIsPartOf10.1002/pola.217972020-06-09T15:59:51Z2006-12-152006-12-15T00:00:00ZHandlehttp://hdl.handle.net/10400.21/11810http://purl.org/coar/access_right/c_16ecrestricted accessCalixareneCatalysisConjugated polymersCyclopolymerizationRhodiumSonogashira coupling452625 bytesliteraturehttp://purl.org/coar/resource_type/c_6501journal articlehttp://purl.org/coar/access_right/c_16ecapplication/pdffulltexthttps://repositorio.ipl.pt/bitstreams/bc7f077f-4c8d-4847-bde5-0954548c1046/downloadJournal of Polymer Science Part A: Polymer Chemistry442470547070
spellingShingle Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers
Costa, Alexandra I.
Calixarene
Catalysis
Conjugated polymers
Cyclopolymerization
Rhodium
Sonogashira coupling
status SINGLETON
subject.fl_str_mv Calixarene
Catalysis
Conjugated polymers
Cyclopolymerization
Rhodium
Sonogashira coupling
title Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers
title_full Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers
title_fullStr Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers
title_full_unstemmed Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers
title_short Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers
title_sort Synthesis and Rh(I)‐catalyzed polymerization of 1,3‐diphenylyne–calix[4]arene compounds: novel conjugated, calixarene‐based polymers
topic Calixarene
Catalysis
Conjugated polymers
Cyclopolymerization
Rhodium
Sonogashira coupling
topic_facet Calixarene
Catalysis
Conjugated polymers
Cyclopolymerization
Rhodium
Sonogashira coupling
url http://hdl.handle.net/10400.21/11810
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