Synthesis of C-tetra(aryl)resorcin[4]arenes using various types of catalysts under solvent free conditions: a comparative study

A comparative study was carried out between the methods of synthesis of C-tetra(aryl)calix[4]resorcinarenes: by means of reflux, that is to say, carrying out a cyclocondensation reaction catalyzed by hydrochloric acid between resorcinol and different aromatic aldehydes, and by means of the solvent-f...

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Main Authors: Carlos Matiz, Alver Castillo-Aguirre, Mauricio Maldonado
Format: Article
Language:English
Published: Taylor & Francis Group 2024-12-01
Series:Green Chemistry Letters and Reviews
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Online Access:https://www.tandfonline.com/doi/10.1080/17518253.2023.2290847
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author Carlos Matiz
Alver Castillo-Aguirre
Mauricio Maldonado
author_facet Carlos Matiz
Alver Castillo-Aguirre
Mauricio Maldonado
author_sort Carlos Matiz
collection DOAJ
description A comparative study was carried out between the methods of synthesis of C-tetra(aryl)calix[4]resorcinarenes: by means of reflux, that is to say, carrying out a cyclocondensation reaction catalyzed by hydrochloric acid between resorcinol and different aromatic aldehydes, and by means of the solvent-free method, which is part of the green chemistry methodologies, in which several catalysts were used, viz. p-toluenesulfonic acid, clinoptilolite zeolite, and silica-gel. In the calix[4]resorcinarenes obtained by both methodologies, mainly 2 types of conformers, crown and chair, were observed. The conformers were isolated and characterized via different spectroscopy techniques: FT-IR, HPLC/MS, 1H-NMR, and 13C-NMR. In these solvent-free and reflux reactions, different ratios were obtained for each of the conformers, finding diverse and unexpected ratios for the solvent-free method. On the other hand, for the solvent-free method there was a significant saving of solvent, an important factor in the care of the environment, as well as of energy and time, in addition to minimizing the significant risks involved in the handling of strong mineral acids.
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spelling doaj-art-693ddf61af754367901a9e3ebdd129e42025-08-20T02:36:09ZengTaylor & Francis GroupGreen Chemistry Letters and Reviews1751-82531751-71922024-12-0117110.1080/17518253.2023.2290847Synthesis of C-tetra(aryl)resorcin[4]arenes using various types of catalysts under solvent free conditions: a comparative studyCarlos Matiz0Alver Castillo-Aguirre1Mauricio Maldonado2Department of chemistry, Universidad Nacional de Colombia, Bogotá, ColombiaDepartment of chemistry, Universidad Nacional de Colombia, Bogotá, ColombiaDepartment of chemistry, Universidad Nacional de Colombia, Bogotá, ColombiaA comparative study was carried out between the methods of synthesis of C-tetra(aryl)calix[4]resorcinarenes: by means of reflux, that is to say, carrying out a cyclocondensation reaction catalyzed by hydrochloric acid between resorcinol and different aromatic aldehydes, and by means of the solvent-free method, which is part of the green chemistry methodologies, in which several catalysts were used, viz. p-toluenesulfonic acid, clinoptilolite zeolite, and silica-gel. In the calix[4]resorcinarenes obtained by both methodologies, mainly 2 types of conformers, crown and chair, were observed. The conformers were isolated and characterized via different spectroscopy techniques: FT-IR, HPLC/MS, 1H-NMR, and 13C-NMR. In these solvent-free and reflux reactions, different ratios were obtained for each of the conformers, finding diverse and unexpected ratios for the solvent-free method. On the other hand, for the solvent-free method there was a significant saving of solvent, an important factor in the care of the environment, as well as of energy and time, in addition to minimizing the significant risks involved in the handling of strong mineral acids.https://www.tandfonline.com/doi/10.1080/17518253.2023.2290847CyclocondensationSolvent-freeChair conformationCrown conformationCatalysis
spellingShingle Carlos Matiz
Alver Castillo-Aguirre
Mauricio Maldonado
Synthesis of C-tetra(aryl)resorcin[4]arenes using various types of catalysts under solvent free conditions: a comparative study
Green Chemistry Letters and Reviews
Cyclocondensation
Solvent-free
Chair conformation
Crown conformation
Catalysis
title Synthesis of C-tetra(aryl)resorcin[4]arenes using various types of catalysts under solvent free conditions: a comparative study
title_full Synthesis of C-tetra(aryl)resorcin[4]arenes using various types of catalysts under solvent free conditions: a comparative study
title_fullStr Synthesis of C-tetra(aryl)resorcin[4]arenes using various types of catalysts under solvent free conditions: a comparative study
title_full_unstemmed Synthesis of C-tetra(aryl)resorcin[4]arenes using various types of catalysts under solvent free conditions: a comparative study
title_short Synthesis of C-tetra(aryl)resorcin[4]arenes using various types of catalysts under solvent free conditions: a comparative study
title_sort synthesis of c tetra aryl resorcin 4 arenes using various types of catalysts under solvent free conditions a comparative study
topic Cyclocondensation
Solvent-free
Chair conformation
Crown conformation
Catalysis
url https://www.tandfonline.com/doi/10.1080/17518253.2023.2290847
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AT alvercastilloaguirre synthesisofctetraarylresorcin4arenesusingvarioustypesofcatalystsundersolventfreeconditionsacomparativestudy
AT mauriciomaldonado synthesisofctetraarylresorcin4arenesusingvarioustypesofcatalystsundersolventfreeconditionsacomparativestudy