Process intensification based on micro reactor technology allows safe manner and a new pathway to... more Process intensification based on micro reactor technology allows safe manner and a new pathway to run organic synthesis due to its intrinsic characteristics, and can reduce time-to-market of new drugs. The main objective of this work was to study the batch and flow reaction of five n-substituted 5-benzylidenethiazolidine-2,4-dione heterocyclic intermediates present in the synthesis of glitazone class drugs, in capillary micro reactor. Batch process was conducted with ethanol as solvent at the boiling point and pyrrolidine as promoting base of the reaction. Higher yields were obtained in shorter reaction times in temperatures above solvent boiling point. Also, we evaluated that 3.8 micro reactors in parallel would be necessary to reach the same mean molar flow rate of a 60 mL batch reactor. Kinetic and thermodynamic study indicated that the reaction followed the second-order model and allowed estimating its main thermodynamic parameters. The continuous flow micro reactor proved to be...
Brazilian Journal of Pharmaceutical Sciences, 2015
This study aims at developing an analytical procedure capable of quantifying the ferric oxide pre... more This study aims at developing an analytical procedure capable of quantifying the ferric oxide present in the mixture of ferric oxide/lactose monohydrate (0.4% w/w). The analytical procedure was checked for specificity, linearity, precision (system repeatability, procedure repeatability and intermediate precision), accuracy, stability of solutions and robustness of the procedure. The concentration of Fe (III) was determined by spectrophotometry at 480 nm based on calibration curves. The specificity was verified. The linearity was obtained in the range of 11.2 to 16.8 µg of ferric oxide/mL. The relative standard deviation (RSD) of the system repeatability, procedure repeatability and intermediate precision, were not more than 2%. The RSD of the accuracy values were less than 0.75%. The stability of the samples was checked over a 24 hours assay. In the robustness evaluation, the wavelength and the concentration of hydrochloric acid varied. The maximum absorbance deviation due to wavele...
Microreactor technology is increasingly applied in the chemical-pharmaceutical industry for safer... more Microreactor technology is increasingly applied in the chemical-pharmaceutical industry for safer and more efficient drug production as compared to the traditional batch process. This technology is employed for the first time to study the production of 2-[methyl(pyridin-2-yl)amino]ethanol, the first intermediate in rosiglitazone synthesis. Under the optimum operating conditions, a single microreactor chip at 160 \ub0C allowed to produce the equivalent of more than five batch reactors at 120 \ub0C. The kinetic study indicated that the reaction is second order. Thermodynamic parameters were determined by the Eyring equation and density functional theory (DFT) calculations with good agreement. DFT results suggested a concerted nucleophilic aromatic substitution reaction mechanism
Reactive Red 141 (RR141) is a diazo reactive dye with bright red color, high molecular weight (1,... more Reactive Red 141 (RR141) is a diazo reactive dye with bright red color, high molecular weight (1,774.15 g/mol), large molecular structure (C52H26Cl2N14Na8O26S8), and several reactive groups. It is ...
Journal of the Taiwan Institute of Chemical Engineers, 2020
The SARS-CoV-2 virus, promoter of COVID-19, already infected millions of people around the world,... more The SARS-CoV-2 virus, promoter of COVID-19, already infected millions of people around the world, resulting in thousands of fatal victims. Facing this unprecedented crisis in human history, several research groups, industrial companies and governments have been spending efforts to develop vaccines and medications. People from distinct knowledge fields are doing their part in order to overcome this crisis. Chemical Engineers are also contributing in the development of actions to control the SARS-CoV-2 virus. However, many chemical engineers still do not know how to use the knowledge acquired from Chemical Engineering school to collaborate in the fight against the COVID-19. In this context, the present paper aims to discuss several knowledge fields within the Chemical Engineering and correlated areas successfully applied to create innovative and effective solutions in the fight against the COVID-19.
The use of microreactors in chemical and pharmaceutical industries allow a series of advantages d... more The use of microreactors in chemical and pharmaceutical industries allow a series of advantages due to their reduced sizes regarding conventional batch reactors. In the present paper the transposition of the reaction between 2,4-Thiazolidinedione with p-Methoxybenzaldehyde, generating the compound with potential biological action against diabetes mellitus type II, from batch to a continuous capillary microreactor was carried out. The microdevice performance was evaluated experimentally and numerically by Computational Fluid Dynamics. The efficiency and viability of microreactors usage for the intermediate pharmaceutical active production was assessed. The optimized operating conditions were obtained for the batch reactor (processing time) and microreactor (residence time), the promoter base selection and optimal concentration was also performed, in order to maximize reactants conversion and reaction yield. Considering the acquired data, computational fluid dynamic simulations were c...
Environmental Engineering and Management Journal, 2015
Chitosan and keratin were tested as low cost biosorbents to remove phenol from water solutions at... more Chitosan and keratin were tested as low cost biosorbents to remove phenol from water solutions at variable temperature (20-50°C), initial phenol concentration (10-90 mg L-1) and pH (5.0-10.0), and fixed biosorbent dosage (10 g L-1). The pseudo-second order kinetic model exhibited the best fit to the experimental data and allowed estimating theoretical values of sorption capacity of 4.51 mg g-1 with keratin and 2.87 mg g-1 with chitosan. Equilibrium isotherms, described at best by the Freundlich model, pointed out that keratin (K F = 1.34 mg 1-1/n L 1/n g-1) was more effective than chitosan (K F = 0.19 mg 1-1/n L 1/n g-1) in phenol removal, although the sorption intensity was almost coincident (n = 1.18-1.19). The results of tests performed at different temperatures suggested a novel thermodynamic approach based on the occurrence of a sorbent inactivation equilibrium, whose changes of enthalpy and entropy were estimated to be 35.7 kJ mol-1 and 118 J mol-1 K-1 with chitosan, and 256 kJ mol-1 and 845 J mol-1 K-1 with keratin. The main functional groups involved in phenol sorption by both raw and phenol-bound materials were identified by FT-IR spectroscopy.
This article has been accepted for publication and undergone full peer review but has not been th... more This article has been accepted for publication and undergone full peer review but has not been through the copyediting, typesetting, pagination and proofreading process, which may lead to differences between this version and the final Version of Record (VOR). This work is currently citable by using the Digital Object Identifier (DOI) given below. The final VoR will be published online in Early View as soon as possible and may be different to this Accepted Article as a result of editing. Readers should obtain the final VoR from the journal website shown below when it is published to ensure accuracy of information. The authors are responsible for the content of this Accepted Article.
This article has been accepted for publication and undergone full peer review but has not been th... more This article has been accepted for publication and undergone full peer review but has not been through the copyediting, typesetting, pagination and proofreading process, which may lead to differences between this version and the final Version of Record (VOR). This work is currently citable by using the Digital Object Identifier (DOI) given below. The final VoR will be published online in Early View as soon as possible and may be different to this Accepted Article as a result of editing. Readers should obtain the final VoR from the journal website shown below when it is published to ensure accuracy of information. The authors are responsible for the content of this Accepted Article.
This article has been accepted for publication and undergone full peer review but has not been th... more This article has been accepted for publication and undergone full peer review but has not been through the copyediting, typesetting, pagination and proofreading process, which may lead to differences between this version and the final Version of Record (VOR). This work is currently citable by using the Digital Object Identifier (DOI) given below. The final VoR will be published online in Early View as soon as possible and may be different to this Accepted Article as a result of editing. Readers should obtain the final VoR from the journal website shown below when it is published to ensure accuracy of information. The authors are responsible for the content of this Accepted Article.
RESUMO-A Pioglitazona é um fármaco usado para o tratamento de diabetes mellitus tipo 2. O present... more RESUMO-A Pioglitazona é um fármaco usado para o tratamento de diabetes mellitus tipo 2. O presente trabalho teve como objetivo a realização de três etapas da síntese do fármaco Pioglitazona. A síntese foi feita em batelada e ao final de cada etapa foram coletadas amostras que posteriormente foram analisadas em HPLC-MS. As análises comprovaram a identidade dos produtos com m/z 229,95 (M+) para a reação I, m/z 256,02 (M+) para a reação II e m/z 357.02 (M+) para a reação III.
Process intensification based on micro reactor technology allows safe manner and a new pathway to... more Process intensification based on micro reactor technology allows safe manner and a new pathway to run organic synthesis due to its intrinsic characteristics, and can reduce time-to-market of new drugs. The main objective of this work was to study the batch and flow reaction of five n-substituted 5-benzylidenethiazolidine-2,4-dione heterocyclic intermediates present in the synthesis of glitazone class drugs, in capillary micro reactor. Batch process was conducted with ethanol as solvent at the boiling point and pyrrolidine as promoting base of the reaction. Higher yields were obtained in shorter reaction times in temperatures above solvent boiling point. Also, we evaluated that 3.8 micro reactors in parallel would be necessary to reach the same mean molar flow rate of a 60 mL batch reactor. Kinetic and thermodynamic study indicated that the reaction followed the second-order model and allowed estimating its main thermodynamic parameters. The continuous flow micro reactor proved to be...
Brazilian Journal of Pharmaceutical Sciences, 2015
This study aims at developing an analytical procedure capable of quantifying the ferric oxide pre... more This study aims at developing an analytical procedure capable of quantifying the ferric oxide present in the mixture of ferric oxide/lactose monohydrate (0.4% w/w). The analytical procedure was checked for specificity, linearity, precision (system repeatability, procedure repeatability and intermediate precision), accuracy, stability of solutions and robustness of the procedure. The concentration of Fe (III) was determined by spectrophotometry at 480 nm based on calibration curves. The specificity was verified. The linearity was obtained in the range of 11.2 to 16.8 µg of ferric oxide/mL. The relative standard deviation (RSD) of the system repeatability, procedure repeatability and intermediate precision, were not more than 2%. The RSD of the accuracy values were less than 0.75%. The stability of the samples was checked over a 24 hours assay. In the robustness evaluation, the wavelength and the concentration of hydrochloric acid varied. The maximum absorbance deviation due to wavele...
Microreactor technology is increasingly applied in the chemical-pharmaceutical industry for safer... more Microreactor technology is increasingly applied in the chemical-pharmaceutical industry for safer and more efficient drug production as compared to the traditional batch process. This technology is employed for the first time to study the production of 2-[methyl(pyridin-2-yl)amino]ethanol, the first intermediate in rosiglitazone synthesis. Under the optimum operating conditions, a single microreactor chip at 160 \ub0C allowed to produce the equivalent of more than five batch reactors at 120 \ub0C. The kinetic study indicated that the reaction is second order. Thermodynamic parameters were determined by the Eyring equation and density functional theory (DFT) calculations with good agreement. DFT results suggested a concerted nucleophilic aromatic substitution reaction mechanism
Reactive Red 141 (RR141) is a diazo reactive dye with bright red color, high molecular weight (1,... more Reactive Red 141 (RR141) is a diazo reactive dye with bright red color, high molecular weight (1,774.15 g/mol), large molecular structure (C52H26Cl2N14Na8O26S8), and several reactive groups. It is ...
Journal of the Taiwan Institute of Chemical Engineers, 2020
The SARS-CoV-2 virus, promoter of COVID-19, already infected millions of people around the world,... more The SARS-CoV-2 virus, promoter of COVID-19, already infected millions of people around the world, resulting in thousands of fatal victims. Facing this unprecedented crisis in human history, several research groups, industrial companies and governments have been spending efforts to develop vaccines and medications. People from distinct knowledge fields are doing their part in order to overcome this crisis. Chemical Engineers are also contributing in the development of actions to control the SARS-CoV-2 virus. However, many chemical engineers still do not know how to use the knowledge acquired from Chemical Engineering school to collaborate in the fight against the COVID-19. In this context, the present paper aims to discuss several knowledge fields within the Chemical Engineering and correlated areas successfully applied to create innovative and effective solutions in the fight against the COVID-19.
The use of microreactors in chemical and pharmaceutical industries allow a series of advantages d... more The use of microreactors in chemical and pharmaceutical industries allow a series of advantages due to their reduced sizes regarding conventional batch reactors. In the present paper the transposition of the reaction between 2,4-Thiazolidinedione with p-Methoxybenzaldehyde, generating the compound with potential biological action against diabetes mellitus type II, from batch to a continuous capillary microreactor was carried out. The microdevice performance was evaluated experimentally and numerically by Computational Fluid Dynamics. The efficiency and viability of microreactors usage for the intermediate pharmaceutical active production was assessed. The optimized operating conditions were obtained for the batch reactor (processing time) and microreactor (residence time), the promoter base selection and optimal concentration was also performed, in order to maximize reactants conversion and reaction yield. Considering the acquired data, computational fluid dynamic simulations were c...
Environmental Engineering and Management Journal, 2015
Chitosan and keratin were tested as low cost biosorbents to remove phenol from water solutions at... more Chitosan and keratin were tested as low cost biosorbents to remove phenol from water solutions at variable temperature (20-50°C), initial phenol concentration (10-90 mg L-1) and pH (5.0-10.0), and fixed biosorbent dosage (10 g L-1). The pseudo-second order kinetic model exhibited the best fit to the experimental data and allowed estimating theoretical values of sorption capacity of 4.51 mg g-1 with keratin and 2.87 mg g-1 with chitosan. Equilibrium isotherms, described at best by the Freundlich model, pointed out that keratin (K F = 1.34 mg 1-1/n L 1/n g-1) was more effective than chitosan (K F = 0.19 mg 1-1/n L 1/n g-1) in phenol removal, although the sorption intensity was almost coincident (n = 1.18-1.19). The results of tests performed at different temperatures suggested a novel thermodynamic approach based on the occurrence of a sorbent inactivation equilibrium, whose changes of enthalpy and entropy were estimated to be 35.7 kJ mol-1 and 118 J mol-1 K-1 with chitosan, and 256 kJ mol-1 and 845 J mol-1 K-1 with keratin. The main functional groups involved in phenol sorption by both raw and phenol-bound materials were identified by FT-IR spectroscopy.
This article has been accepted for publication and undergone full peer review but has not been th... more This article has been accepted for publication and undergone full peer review but has not been through the copyediting, typesetting, pagination and proofreading process, which may lead to differences between this version and the final Version of Record (VOR). This work is currently citable by using the Digital Object Identifier (DOI) given below. The final VoR will be published online in Early View as soon as possible and may be different to this Accepted Article as a result of editing. Readers should obtain the final VoR from the journal website shown below when it is published to ensure accuracy of information. The authors are responsible for the content of this Accepted Article.
This article has been accepted for publication and undergone full peer review but has not been th... more This article has been accepted for publication and undergone full peer review but has not been through the copyediting, typesetting, pagination and proofreading process, which may lead to differences between this version and the final Version of Record (VOR). This work is currently citable by using the Digital Object Identifier (DOI) given below. The final VoR will be published online in Early View as soon as possible and may be different to this Accepted Article as a result of editing. Readers should obtain the final VoR from the journal website shown below when it is published to ensure accuracy of information. The authors are responsible for the content of this Accepted Article.
This article has been accepted for publication and undergone full peer review but has not been th... more This article has been accepted for publication and undergone full peer review but has not been through the copyediting, typesetting, pagination and proofreading process, which may lead to differences between this version and the final Version of Record (VOR). This work is currently citable by using the Digital Object Identifier (DOI) given below. The final VoR will be published online in Early View as soon as possible and may be different to this Accepted Article as a result of editing. Readers should obtain the final VoR from the journal website shown below when it is published to ensure accuracy of information. The authors are responsible for the content of this Accepted Article.
RESUMO-A Pioglitazona é um fármaco usado para o tratamento de diabetes mellitus tipo 2. O present... more RESUMO-A Pioglitazona é um fármaco usado para o tratamento de diabetes mellitus tipo 2. O presente trabalho teve como objetivo a realização de três etapas da síntese do fármaco Pioglitazona. A síntese foi feita em batelada e ao final de cada etapa foram coletadas amostras que posteriormente foram analisadas em HPLC-MS. As análises comprovaram a identidade dos produtos com m/z 229,95 (M+) para a reação I, m/z 256,02 (M+) para a reação II e m/z 357.02 (M+) para a reação III.
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