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Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling

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Resumo:The aim of this work is the synthesis of a formyl-arylthiophene derivative, using simple experimental techniques and commercially available reagents. The synthesis of this compound involves a palladium catalysed cross-coupling reaction (Suzuki-Miyaura coupling), between a boronic acid derivative and a heterocyclic brominated compound using DME as solvent and Na2CO3 as base. Different coupling components would be used in order to determine the influence of the structure of the boronic acid as well as the brominated compound on the yield of the Suzuki-Miyaura coupling reaction. Several experimental techniques will be considered such as heating at reflux under an inert atmosphere, liquid-liquid extraction, gravity and vacuum filtration, thin layer chromatography (TLC), column chromatography on silica gel and melting point. The determination of the structure of the compound synthesized will be also performed through 1H NMR and IR spectroscopic techniques. The duration of the experiment will be 3 sessions: session 1: preparation of 5-phenylthiophene-2-carbaldehyde; session 2: isolation of 5-phenylthiophene-2-carbaldehyde; session 3: purification of 5-phenylthiophene-2-carbaldehyde using column chromatography on silica gel. The difficulty level of this experiment is medium and the level of study is intermediate.
Autores principais:Raposo, M. Manuela M.
Outros Autores:Costa, Susana P. G.; Batista, Rosa Maria Ferreira; Ferreira, Rosa Cristina Moutinho
Assunto:Chromatography NMR Suzuki-Miyaura cross-coupling Thiophene Boronic acid Aldehyde Synthesis Reactivity studies Organic Chemistry Experiments Laboratory Classroom Ciências Naturais::Ciências Químicas
Ano:2016
País:Portugal
Tipo de documento:capítulo de livro
Tipo de acesso:acesso restrito
Instituição associada:Universidade do Minho
Idioma:inglês
Origem:RepositóriUM - Universidade do Minho
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author Raposo, M. Manuela M.
author2 Costa, Susana P. G.
Batista, Rosa Maria Ferreira
Ferreira, Rosa Cristina Moutinho
author2_role author
author
author
author_facet Raposo, M. Manuela M.
Costa, Susana P. G.
Batista, Rosa Maria Ferreira
Ferreira, Rosa Cristina Moutinho
author_role author
contributor_name_str_mv RepositóriUM - Universidade do Minho
country_str PT
creators_json_txt [{\"Person.name\":\"Raposo, M. Manuela M.\"},{\"Person.name\":\"Costa, Susana P. G.\"},{\"Person.name\":\"Batista, Rosa Maria Ferreira\"},{\"Person.name\":\"Ferreira, Rosa Cristina Moutinho\"}]
datacite.contributors.contributor.contributorName.fl_str_mv RepositóriUM - Universidade do Minho
datacite.creators.creator.creatorName.fl_str_mv Raposo, M. Manuela M.
Costa, Susana P. G.
Batista, Rosa Maria Ferreira
Ferreira, Rosa Cristina Moutinho
datacite.date.Accepted.fl_str_mv 2016-01-01T00:00:00Z
datacite.rights.fl_str_mv http://purl.org/coar/access_right/c_16ec
datacite.subjects.subject.fl_str_mv Chromatography
NMR
Suzuki-Miyaura cross-coupling
Thiophene
Boronic acid
Aldehyde
Synthesis
Reactivity studies
Organic Chemistry Experiments
Laboratory Classroom
Ciências Naturais::Ciências Químicas
datacite.titles.title.fl_str_mv Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling
dc.contributor.none.fl_str_mv RepositóriUM - Universidade do Minho
dc.creator.none.fl_str_mv Raposo, M. Manuela M.
Costa, Susana P. G.
Batista, Rosa Maria Ferreira
Ferreira, Rosa Cristina Moutinho
dc.date.Accepted.fl_str_mv 2016-01-01T00:00:00Z
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.identifier.none.fl_str_mv https://hdl.handle.net/1822/49427
dc.language.none.fl_str_mv eng
dc.publisher.none.fl_str_mv Royal Society of Chemistry
dc.rights.cclincense.fl_str_mv http://creativecommons.org/licenses/by/4.0/
dc.rights.none.fl_str_mv http://purl.org/coar/access_right/c_16ec
dc.rights.rights.copyright.fl_str_mv closedAccess
dc.subject.none.fl_str_mv Chromatography
NMR
Suzuki-Miyaura cross-coupling
Thiophene
Boronic acid
Aldehyde
Synthesis
Reactivity studies
Organic Chemistry Experiments
Laboratory Classroom
Ciências Naturais::Ciências Químicas
dc.title.fl_str_mv Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling
dc.type.none.fl_str_mv http://purl.org/coar/resource_type/c_3248
description The aim of this work is the synthesis of a formyl-arylthiophene derivative, using simple experimental techniques and commercially available reagents. The synthesis of this compound involves a palladium catalysed cross-coupling reaction (Suzuki-Miyaura coupling), between a boronic acid derivative and a heterocyclic brominated compound using DME as solvent and Na2CO3 as base. Different coupling components would be used in order to determine the influence of the structure of the boronic acid as well as the brominated compound on the yield of the Suzuki-Miyaura coupling reaction. Several experimental techniques will be considered such as heating at reflux under an inert atmosphere, liquid-liquid extraction, gravity and vacuum filtration, thin layer chromatography (TLC), column chromatography on silica gel and melting point. The determination of the structure of the compound synthesized will be also performed through 1H NMR and IR spectroscopic techniques. The duration of the experiment will be 3 sessions: session 1: preparation of 5-phenylthiophene-2-carbaldehyde; session 2: isolation of 5-phenylthiophene-2-carbaldehyde; session 3: purification of 5-phenylthiophene-2-carbaldehyde using column chromatography on silica gel. The difficulty level of this experiment is medium and the level of study is intermediate.
dirty 0
eu_rights_str_mv restrictedAccess
format bookPart
fulltext.url.fl_str_mv https://repositorium.uminho.pt/bitstreams/1f125392-7c9d-4d5d-a01d-94f5d5e83fc1/download
id rum_d7ec00b6ff197a9496b4c7b072a2ca13
identifier.url.fl_str_mv https://hdl.handle.net/1822/49427
instacron_str repositorium
institution Universidade do Minho
instname_str Universidade do Minho
language eng
network_acronym_str rum
network_name_str RepositóriUM - Universidade do Minho
oai_identifier_str oai:repositorium.uminho.pt:1822/49427
organization_str_mv urn:organizationAcronym:repositorium
person_str_mv Raposo, M. Manuela M.
Costa, Susana P. G.
Batista, Rosa Maria Ferreira
Ferreira, Rosa Cristina Moutinho
publishDate 2016
publisher.none.fl_str_mv Royal Society of Chemistry
reponame_str RepositóriUM - Universidade do Minho
repository_id_str urn:repositoryAcronym:rum
service_str_mv urn:repositoryAcronym:rum
spelling engRoyal Society of ChemistryporThe aim of this work is the synthesis of a formyl-arylthiophene derivative, using simple experimental techniques and commercially available reagents. The synthesis of this compound involves a palladium catalysed cross-coupling reaction (Suzuki-Miyaura coupling), between a boronic acid derivative and a heterocyclic brominated compound using DME as solvent and Na2CO3 as base. Different coupling components would be used in order to determine the influence of the structure of the boronic acid as well as the brominated compound on the yield of the Suzuki-Miyaura coupling reaction. Several experimental techniques will be considered such as heating at reflux under an inert atmosphere, liquid-liquid extraction, gravity and vacuum filtration, thin layer chromatography (TLC), column chromatography on silica gel and melting point. The determination of the structure of the compound synthesized will be also performed through 1H NMR and IR spectroscopic techniques. The duration of the experiment will be 3 sessions: session 1: preparation of 5-phenylthiophene-2-carbaldehyde; session 2: isolation of 5-phenylthiophene-2-carbaldehyde; session 3: purification of 5-phenylthiophene-2-carbaldehyde using column chromatography on silica gel. The difficulty level of this experiment is medium and the level of study is intermediate.application/pdfapplication/pdfporReactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura couplingRaposo, M. Manuela M.Costa, Susana P. G.Batista, Rosa Maria FerreiraFerreira, Rosa Cristina MoutinhoHostingInstitutionOrganizationalRepositóriUM - Universidade do Minhoe-mailmailto:repositorium@usdb.uminho.ptrepositorium@usdb.uminho.ptCITATIONRaposo, M. M. M.; Costa, S. P. G.: Batista, R. M. F.; Ferreira, R. C. M. in Comprehensive Organic Chemistry Experiments for the Laboratory Classroom (COCELC), “Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling”, Afonso, C. A. M.; Franzén, R.; Tan, B.; Candeias, N. R.; Simão, D.; Trindade, A.; Coelho, J. (Eds); Royal Society of Chemistry 2016, Chapter 142, Experiment 7.2., p 628-632 (ISBN 978-18-49739-63-4).ISBNIsPartOf978-18-49739-63-420162016-01-01T00:00:00ZHandlehttps://hdl.handle.net/1822/49427http://purl.org/coar/access_right/c_16ecrestricted accessChromatographyNMRSuzuki-Miyaura cross-couplingThiopheneBoronic acidAldehydeSynthesisReactivity studiesOrganic Chemistry ExperimentsLaboratory Classroomhttp://www.oecd.org/science/inno/38235147.pdfFields of Science and Technology (FOS)Ciências Naturais::Ciências Químicas254410 bytes399491 bytesliteraturehttp://purl.org/coar/resource_type/c_3248book part2016http://creativecommons.org/licenses/by/4.0/closedAccesshttp://purl.org/coar/access_right/c_16ecapplication/pdffulltexthttps://repositorium.uminho.pt/bitstreams/1f125392-7c9d-4d5d-a01d-94f5d5e83fc1/downloadhttp://purl.org/coar/access_right/c_16ecapplication/pdffulltexthttps://repositorium.uminho.pt/bitstreams/b818fcea-def0-4d22-8935-bef02de523cd/download
spellingShingle Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling
Raposo, M. Manuela M.
Chromatography
NMR
Suzuki-Miyaura cross-coupling
Thiophene
Boronic acid
Aldehyde
Synthesis
Reactivity studies
Organic Chemistry Experiments
Laboratory Classroom
Ciências Naturais::Ciências Químicas
status SINGLETON
subject.fl_str_mv Chromatography
NMR
Suzuki-Miyaura cross-coupling
Thiophene
Boronic acid
Aldehyde
Synthesis
Reactivity studies
Organic Chemistry Experiments
Laboratory Classroom
subject.other.fl_str_mv Ciências Naturais::Ciências Químicas
title Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling
title_full Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling
title_fullStr Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling
title_full_unstemmed Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling
title_short Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling
title_sort Reactivity studies for the synthesis of 5-phenylthiophene-2-carbaldehyde by Suzuki-Miyaura coupling
topic Chromatography
NMR
Suzuki-Miyaura cross-coupling
Thiophene
Boronic acid
Aldehyde
Synthesis
Reactivity studies
Organic Chemistry Experiments
Laboratory Classroom
Ciências Naturais::Ciências Químicas
topic_facet Chromatography
NMR
Suzuki-Miyaura cross-coupling
Thiophene
Boronic acid
Aldehyde
Synthesis
Reactivity studies
Organic Chemistry Experiments
Laboratory Classroom
Ciências Naturais::Ciências Químicas
url https://hdl.handle.net/1822/49427
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