Effect of the Titanium Isopropoxide:Acetylacetone Molar Ratio on the Photocatalytic Activity of Tio2 Thin Films
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Synthesis and Antimicrobial Evaluation of Some Novel Thiazole, Pyridone, Pyrazole, Chromene, Hydrazone Derivatives Bearing a Biologically Active Sulfonamide Moiety
Int. J. Mol. Sci. 2014, 15, 1237-1254; doi:10.3390/ijms15011237 OPEN ACCESS International Journal of Molecular Sciences ISSN 1422-0067 www.mdpi.com/journal/ijms Article Synthesis and Antimicrobial Evaluation of Some Novel Thiazole, Pyridone, Pyrazole, Chromene, Hydrazone Derivatives Bearing a Biologically Active Sulfonamide Moiety Elham S. Darwish *, Azza M. Abdel Fattah, Fawzy A. Attaby and Oqba N. Al-Shayea Department of Chemistry, Faculty of Science, Cairo University, Giza 12613, Egypt; E-Mails: [email protected] (A.M.A.F.); [email protected] (F.A.A.); [email protected] (O.N.A.-S.) * Author to whom correspondence should be addressed; E-Mail: [email protected]; Tel.: +20-100-588-1771; Fax: +202-570-8480. Received: 10 November 2013; in revised form: 10 January 2014 / Accepted: 13 January 2014 / Published: 17 January 2014 Abstract: This study aimed for the synthesis of new heterocyclic compounds incorporating sulfamoyl moiety suitable for use as antimicrobial agents via a versatile, readily accessible N-[4-(aminosulfonyl)phenyl]-2-cyanoacetamide (3). The 2-pyridone derivatives were obtained via reaction of cyanoacetamide with acetylacetone or arylidenes malononitrile. Cycloaddition reaction of cyanoacetamide with salicyaldehyde furnished chromene derivatives. Diazotization of 3 with the desired diazonium chloride gave the hydrazone derivatives 13a–e. Also, the reactivity of the hydrazone towards hydrazine hydrate to give Pyrazole derivatives was studied. In addition, treatment of 3 with elemental sulfur and phenyl isothiocyanate or malononitrile furnished thiazole and thiophene derivatives respectively. Reaction of 3 with phenyl isothiocyanate and KOH in DMF afforded the intermediate salt 17 which reacted in situ with 3-(2-bromoacetyl)-2H-chromen-2-one and methyl iodide afforded the thiazole and ketene N,S-acetal derivatives respectively. -
Brno University of Technology
BRNO UNIVERSITY OF TECHNOLOGY Faculty of Chemistry DOCTORAL THESIS Brno, 2016 Ing. Tomá Solný BRNO UNIVERSITY OF TECHNOLOGY VYSOKÉ UENÍ TECHNICKÉ V BRN FACULTY OF CHEMISTRY FAKULTA CHEMICKÁ INSTITUTE OF MATERIALS SCIENCE ÚSTAV CHEMIE MATERIÁL SYNTHESIS AND PHOTOCATALYTIC APPLICATIONS OF TITANIUM DIOXIDE PÍPRAVA A APLIKACE FOTOKATALYTICKY AKTIVNÍHO OXIDU TITANIITÉHO DOCTORAL THESIS DIZERTANÍ PRÁCE AUTHOR Ing. Tomá Solný AUTOR PRÁCE SUPERVISOR doc. Ing. Petr Ptáek, Ph.D. KOLITEL BRNO 2016 ABSTRACT Hydrolysis conditions for different Ti-alkoxides were examined considering the impact of water to alkoxide ratio and temperature. The prepared hydrolysates and sintered TiO2 nanoparticles were examined with XRD, DTA – TGA, SEM – EDS, BET and PCCS analysis in order to identify the impact of hydrolysis on properties of prepared anatase particles. Magnetite nanoparticles were synthetized by easy one step precipitation method from Mohr´s salt solution and their crystallinity, size and surface properties were examined investigating the influence of temperature and coating by polycarboxylate ether superplasticizer. For immobilization of TiO2 on surfaces of magnetite combined method using the selected nanoparticles of TiO2 and Ti-alkoxides hydrolysis is performed in order to obtain photocatalytically active core–shell powder catalysator with enhanced adsorptive properties. Also the investigation on the applications of TiO2 on surfaces of Mn-Zn ferrite is done with studying the surface treatment by CVD deposition of C and Au layer. Photocatalytic activity of selected prepared photocatalysators is evaluated upon decomposition of methylene blue and isopropanolic and ethanolic vapors for Mn-Zn ferrite in experimental chemical reactor with magnetically holded powdered photocatalysator beds. KEYWORDS: Titanium oxide, anatase, photocatalytic activity, core-shell powder photocatalysator, magnetite, Mn-Zn ferrite, Ti-alkoxides, hydrolysis, sol-gel, nanoparticles. -
Feiii, Cuii and Znii Complexes of the Rigid 9-Oxido-Phenalenone Ligand—Spectroscopy, Electrochemistry, and Cytotoxic Properties
International Journal of Molecular Sciences Article FeIII, CuII and ZnII Complexes of the Rigid 9-Oxido-phenalenone Ligand—Spectroscopy, Electrochemistry, and Cytotoxic Properties Katharina Butsch 1, Alexander Haseloer 1 , Simon Schmitz 1, Ingo Ott 2, Julia Schur 2 and Axel Klein 1,* 1 Department für Chemie, Institut für Anorganische Chemie, Universität zu Köln, Greinstraße 6, D-50939 Köln, Germany; [email protected] (K.B.); [email protected] (A.H.); [email protected] (S.S.) 2 Institute of Medicinal and Pharmaceutical Chemistry, Technische Universität Braunschweig, Beethovenstrasse 55, D-38106 Braunschweig, Germany; [email protected] (I.O.); [email protected] (J.S.) * Correspondence: [email protected] Abstract: The three complexes [Fe(opo)3], [Cu(opo)2], and [Zn(opo)2] containing the non-innocent anionic ligand opo− (opo− = 9-oxido-phenalenone, Hopo = 9-hydroxyphenalonone) were synthe- 1 sised from the corresponding acetylacetonates. [Zn(opo)2] was characterised using H nuclear magnetic resonance (NMR) spectroscopy, the paramagnetic [Fe(opo)3] and [Cu(opo)2] by electron paramagnetic resonance (EPR) spectroscopy. While the EPR spectra of [Cu(opo)2] and [Cu(acac)2] in dimethylformamide (DMF) solution are very similar, a rather narrow spectrum was observed for [Fe(opo)3] in tetrahydrofuran (THF) solution in contrast to the very broad spectrum of [Fe(acac)3] in − Citation: Butsch, K.; Haseloer, A.; THF (Hacac = acetylacetone, 2,4-pentanedione; acac = acetylacetonate). The narrow, completely Schmitz, S.; Ott, I.; Schur, J.; Klein, A. isotropic signal of [Fe(opo)3] disagrees with a metal-centred S = 5/2 spin system that is observed FeIII, CuII and ZnII Complexes of the in the solid state. -
WO 2017/031289 Al 23 February 2017 (23.02.2017) P O P C T
(12) INTERNATIONAL APPLICATION PUBLISHED UNDER THE PATENT COOPERATION TREATY (PCT) (19) World Intellectual Property Organization International Bureau (10) International Publication Number (43) International Publication Date WO 2017/031289 Al 23 February 2017 (23.02.2017) P O P C T (51) International Patent Classification: (81) Designated States (unless otherwise indicated, for every A01N 25/04 (2006.01) A01N 25/24 (2006.01) kind of national protection available): AE, AG, AL, AM, A 59/00 (2006.01) AOIN25/26 (2006.01) AO, AT, AU, AZ, BA, BB, BG, BH, BN, BR, BW, BY, A0 33/12 (2006.01) BZ, CA, CH, CL, CN, CO, CR, CU, CZ, DE, DK, DM, DO, DZ, EC, EE, EG, ES, FI, GB, GD, GE, GH, GM, GT, (21) International Application Number: HN, HR, HU, ID, IL, IN, IR, IS, JP, KE, KG, KN, KP, KR, PCT/US20 16/047509 KZ, LA, LC, LK, LR, LS, LU, LY, MA, MD, ME, MG, (22) International Filing Date: MK, MN, MW, MX, MY, MZ, NA, NG, NI, NO, NZ, OM, 18 August 2016 (18.08.2016) PA, PE, PG, PH, PL, PT, QA, RO, RS, RU, RW, SA, SC, SD, SE, SG, SK, SL, SM, ST, SV, SY, TH, TJ, TM, TN, (25) Filing Language: English TR, TT, TZ, UA, UG, US, UZ, VC, VN, ZA, ZM, ZW. (26) Publication Language: English (84) Designated States (unless otherwise indicated, for every (30) Priority Data: kind of regional protection available): ARIPO (BW, GH, 62/207,750 20 August 2015 (20.08.2015) US GM, KE, LR, LS, MW, MZ, NA, RW, SD, SL, ST, SZ, TZ, UG, ZM, ZW), Eurasian (AM, AZ, BY, KG, KZ, RU, (71) Applicant: INTEGRICOTE, INC. -
Glycosyl Barbiturate Ligands of Bacterial Lectins: from Monomer Design to Glycoclusters and Glycopolymers François Portier, Anne Imberty, Sami Halila
View metadata, citation and similar papers at core.ac.uk brought to you by CORE provided by Archive Ouverte en Sciences de l'Information et de la Communication Expeditious Synthesis of C -Glycosyl Barbiturate Ligands of Bacterial Lectins: From Monomer Design to Glycoclusters and Glycopolymers François Portier, Anne Imberty, Sami Halila To cite this version: François Portier, Anne Imberty, Sami Halila. Expeditious Synthesis of C -Glycosyl Barbiturate Lig- ands of Bacterial Lectins: From Monomer Design to Glycoclusters and Glycopolymers. Bioconjugate Chemistry, American Chemical Society, 2019, 30 (3), pp.647-656. 10.1021/acs.bioconjchem.8b00847. hal-02322076 HAL Id: hal-02322076 https://hal.archives-ouvertes.fr/hal-02322076 Submitted on 4 Aug 2020 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. EXPEDITIOUS SYNTHESIS OF C‐GLYCOSYL BARBITURATE LIGANDS OF BACTERIAL LECTINS: FROM MONOMER DESIGN TO GLYCOCLUSTERS AND GLYCOPOLYMERS François Portier, Anne Imberty and Sami Halila* Univ. Grenoble Alpes, CNRS, CERMAV, 38000 Grenoble, France. E‐mail: [email protected]; Fax: +33 4 76 54 72 03; Tel : +33 4 76 03 76 66 ABSTRACT The approach developed here offers a straightforward and efficient access to ‐C‐glycosyl barbiturates ligands, spanning from glycomimetics to multivalent C‐neoglycoconjugates, with the aim of deciphering structural parameters impacting the binding to pathogenic lectins. -
Synthesis and Characterization of Schiff Bases Derived from Acetylacetone and Their Theoretical Study
International Journal of ChemTech Research CODEN( USA): IJCRGG ISSN : 0974-4290 Vol.5, No.1, pp 204-211, Jan-Mar 2013 Synthesis And Characterization Of Schiff Bases Derived From Acetylacetone And Their Theoretical Study Adnan dib Department of Chemistry, Faculty of Science, Laboratory of Organic Chemistry, University of Damascus, Syria Corres.author: [email protected] Abstract: Schiff basesderived from acetylacetone were synthesized and characterized by Ms, IR, 1H ,13C NMR and element analysis. Hyper Chem-6 program has been used to predict structural geometries of compounds in gas phase. The heat of formation (ΔHf º) and binding energy (ΔEb) at 298 ºK for the free ligand was calculated by PM3 method. Keywords: Schiff bases, acetylacetone, hydrazine, PM3 method. Introduction Experimental Schiff bases are one of the most versatile classes of Reagents and Apparatus. ligands for the study of the coordination of transition All the chemicals used were of AnalaR grade and metals[1]. Their ease of synthesis (by the procured from Sigma-Aldrich and Fluka. Metal salts condensation of an aldehyde/ketone with an amine), were purchased from E. Merck and were used as multidenticity (from mono to hexadentate), received. Distilled water was used in extraction combination of donor atoms (coordination usually experimentals. The solvents were saturated with through the imine nitrogen and other atoms like each other before use in order to prevent volume oxygen, sulfur or nitrogen) and stability have made changes of the phases during extraction. The C, H, them the preferred ligand system in catalysis, and N were analyzed on a Carlo-Erba 1106 biological modeling, the design of molecular elemental analyzer. -
Determination of Solvent Effects on Ketoðenol Equilibria of 1,3-Dicarbonyl Compounds Using NMR: Revisiting a Classic Physical C
In the Laboratory Determination of Solvent Effects on Keto–Enol Equilibria W of 1,3-Dicarbonyl Compounds Using NMR Revisiting a Classic Physical Chemistry Experiment Gilbert Cook* and Paul M. Feltman Department of Chemistry, Valparaiso University, Valparaiso, IN 46383; *[email protected] “The influence of solvents on chemical equilibria was discovered in 1896, simultaneously with the discovery of keto–enol tautomerism in 1,3-dicarbonyl compounds” (1). The solvents were divided into two groups according to their ability to isomerize compounds. The study of the keto–enol tautomerism of β-diketones and β-ketoesters in a variety of solvents using proton NMR has been utilized as a physical Figure 1. The β-dicarbonyl compounds studied in the experiment. chemistry experiment for many years (2, 3). The first reported use of NMR keto–enol equilibria determination was by Reeves (4). This technique has been described in detail in an experiment by Garland, Nibler, and Shoemaker (2). panded (i) to give an in-depth analysis of factors influencing The most commonly used β-diketone for these experi- solvent effects in tautomeric equilibria and (ii) to illustrate ments is acetylacetone (Scheme I). Use of proton NMR is a the use of molecular modeling in determining the origin of viable method for measuring this equilibrium because the a molecule’s polarity. The experiment’s original benefits of tautomeric keto–enol equilibrium is slow on the NMR time using proton NMR as a noninvasive method of evaluating scale, but enol (2a)–enol (2b) tautomerism is fast on this scale equilibrium are maintained. (5). It has been observed that acyclic β-diketones and β- Experimental Procedure ketoesters follow Meyer’s rule of a shift in the tautomeric equi- librium toward the keto tautomer with increasing solvent Observations of the solvent effects for three other 1,3- polarity (6). -
Effect of Titanium Source and Sol-Gel Tio2 Thin Film Formation Parameters
Materials Science-Poland, 38(3), 2020, pp. 424-433 http://www.materialsscience.pwr.wroc.pl/ DOI: 10.2478/msp-2020-0056 Effect of titanium source and sol-gel TiO2 thin film formation parameters on its morphology and photocatalytic activity PIOTR DULIAN∗,JAN ZAJIC,WITOLD Z˙ UKOWSKI Faculty of Chemical Engineering and Technology, Cracow University of Technology, 24 Warszawska St., 310155 Cracow, Poland TiO2 thin films with different surface structure have been prepared from alkoxide solutions by the sol-gel method using different cationic precursors and heat treatment techniques. The effect of using titanium isopropoxide as well as titanium butox- ide as a titanium source on the surface structure and photocatalytic activity of the resultant thin films was studied. Significant differences in the rate of hydrolysis and condensation reactions during the sol-gel synthesis were observed for these titanium precursors. This had a direct influence on the morphology of the as-prepared TiO2 films. Higher quality oxide coatings were obtained from titanium isopropoxide. They were characterized by a smaller grain size, improved surface roughness and uni- form coverage of the glass substrate. A beneficial effect of calcination process after each sol application cycle in contrast to single step calcination after all dip-coating cycles was observed. Photocatalytic degradation tests showed that methyl orange was decolorized in the presence of all prepared TiO2 films by exposing their aqueous solutions to UV light (λ = 254 nm). The highest photocatalytic activity had the TiO2 layer produced using titanium isopropoxide. Keywords: TiO2 thin film; sol-gel; photocatalysis 1. Introduction and corrosion protection [5–12]. Currently, several techniques for producing thin semiconductor lay- Environmental pollution is one of the main ers [13–17] are known. -
Acetylacetone
Safety data sheet acc. to Safe Work Australia - Code of Practice Acetylacetone ≥98 %, for synthesis article number: 6716 date of compilation: 2016-11-08 Version: GHS 2.0 en Revision: 2021-06-11 Replaces version of: 2016-11-08 Version: (GHS 1) SECTION 1: Identification of the substance/mixture and of the company/ undertaking 1.1 Product identifier Identification of the substance Acetylacetone ≥98 %, for synthesis Article number 6716 CAS number 123-54-6 Alternative name(s) Pentane-2,4-dione 1.2 Relevant identified uses of the substance or mixture and uses advised against Relevant identified uses: Laboratory chemical Laboratory and analytical use Uses advised against: Do not use for products which come into contact with foodstuffs. Do not use for private purposes (household). 1.3 Details of the supplier of the safety data sheet Carl Roth GmbH + Co KG Schoemperlenstr. 3-5 D-76185 Karlsruhe Germany Telephone:+49 (0) 721 - 56 06 0 Telefax: +49 (0) 721 - 56 06 149 e-mail: [email protected] Website: www.carlroth.de Competent person responsible for the safety data :Department Health, Safety and Environment sheet: e-mail (competent person): [email protected] 1.4 Emergency telephone number Name Street Postal Telephone Website code/city NSW Poisons Information Centre Hawkesbury Road 2145 West- 131126 Childrens Hospital mead, NSW SECTION 2: Hazards identification 2.1 Classification of the substance or mixture Classification acc. to GHS Section Hazard class Cat- Hazard class and Hazard egory category statement 2.6 Flammable liquid 3 Flam. Liq. 3 H226 3.1O Acute toxicity (oral) 4 Acute Tox. -
Polarography As a Measure of Ionic Environment
University of the Pacific Scholarly Commons University of the Pacific Theses and Dissertations Graduate School 1965 Polarography As A Measure Of Ionic Environment James Wilburne Larsen University of the Pacific Follow this and additional works at: https://scholarlycommons.pacific.edu/uop_etds Part of the Chemistry Commons Recommended Citation Larsen, James Wilburne. (1965). Polarography As A Measure Of Ionic Environment. University of the Pacific, Dissertation. https://scholarlycommons.pacific.edu/uop_etds/2881 This Dissertation is brought to you for free and open access by the Graduate School at Scholarly Commons. It has been accepted for inclusion in University of the Pacific Theses and Dissertations by an authorized administrator of Scholarly Commons. For more information, please contact [email protected]. .. i:' ~)~-~;~::"',:'.,·~-~ -~·-:.·: ~ -~ ·. ,. '~:-··~· ··:.\';~<_; i ~~ .:•i'{O" .1"' POLAROGRAPHY AS A MEASURE OF IONIC ENVIRONMENT A Dissertation _Presented to the Faculty of the Graduate School University of the Pacific In Partial Fulfillment of the Requirements for the Degree (f ' Doctor of Philosophy by James Wilburne Larsen June 1965 This disseljtatic;m,, written apd submitted by is approved for recornrnendat,ipn to the Graduate Co~ncil, University of th~ P~(::.ific • . D~partmept Chairwan or Dean: ACKNOWLEDGEMENTS The writer wishes to express his appreciation to the faculty of the Chemistry Department for their assistance, especially Dr. Herschel Frye for his criticisms and guidance. TABLE OF CONTENTS CHAPTER PAGE I. INTRODUCTION -
Synthesis and Transformation of Hollow Rutile Titania Wires by Single Spinneret Electrospinning with Sol-Gel Chemistry
fibers Article Synthesis and Transformation of Hollow Rutile Titania Wires by Single Spinneret Electrospinning with Sol-Gel Chemistry Chin-Shuo Kang and Edward Evans * Department of Chemical, Biomolecular and Corrosion Engineering, The University of Akron, Akron, OH 44325, USA; [email protected] * Correspondence: [email protected] Abstract: The work described below was carried out to understand how to control the morphology of nanostructured titania calcined from electrospun nanofibers. This is the first report of hollow rutile nanofibers synthesized from electrospun nanofibers with short calcination time. Titanium isopropoxide was incorporated into the nanofibers as the titania precursor. The electrospinning technique was used to fabricate ceramic/polymer hybrid nanofibers. The electrospun nanofibers were then calcined to produce rutile titania nanofibers with different morphologies (hollow or solid nanofibers), which were characterized by SEM and TEM. The initial concentration of ceramic precursor and the calcination time were shown to control the morphology of the nanofiber. The hollow morphology was only obtained with a concentration of the precursor within a certain level and with short calcination times. The heat treatment profile contributed to particle growth. At longer times, the particle growth led to the closure of the hollow core and all the nanofibers resembled strings of solid particles. A formation mechanism for the hollow nanofibers is also proposed. Keywords: electrospinning; TiO2; hollow nanofiber; nanofiber formation Citation: Kang, C.-S.; Evans, E. Synthesis and Transformation of Hollow Rutile Titania Wires by Single 1. Introduction Spinneret Electrospinning with One-dimensional titania nanostructures have been used in different applications based Sol-Gel Chemistry. Fibers 2021, 9, 18. on their morphology. -
Titanium(IV) Isopropoxide
Titanium(IV) isopropoxide sc-253704 Material Safety Data Sheet Hazard Alert Code EXTREME HIGH MODERATE LOW Key: Section 1 - CHEMICAL PRODUCT AND COMPANY IDENTIFICATION PRODUCT NAME Titanium(IV) isopropoxide STATEMENT OF HAZARDOUS NATURE CONSIDERED A HAZARDOUS SUBSTANCE ACCORDING TO OSHA 29 CFR 1910.1200. NFPA FLAMMABILITY3 HEALTH4 HAZARD INSTABILITY0 SUPPLIER Santa Cruz Biotechnology, Inc. 2145 Delaware Avenue Santa Cruz, California 95060 800.457.3801 or 831.457.3800 EMERGENCY ChemWatch Within the US & Canada: 877-715-9305 Outside the US & Canada: +800 2436 2255 (1-800-CHEMCALL) or call +613 9573 3112 SYNONYMS C12-H28-O4-Ti, C3-H8-O.1/4Ti, Ti[OCH(CH3)2]4, "isopropyl orthotitanate", "isopropyl titanate (IV)", tetraisopropoxytitanium, "tetraisopropoxide titanium", "tetraisopropyl orthotitanate", "tetraisopropyl titanate", "tetra isopropyl titanate", "titanium(4+) isopropoxide", "titanium isopropylate", "titanium tetraisopropoxide", "titanium tetraisopropylate", "titanium tetra-n-propoxide" Section 2 - HAZARDS IDENTIFICATION CHEMWATCH HAZARD RATINGS Min Max Flammability 2 Toxicity 2 Min/Nil=0 Low=1 Body Contact 2 Moderate=2 Reactivity 1 High=3 Extreme=4 1 of 16 Chronic 2 CANADIAN WHMIS SYMBOLS EMERGENCY OVERVIEW RISK Harmful by inhalation. Irritating to eyes, respiratory system and skin. Flammable. POTENTIAL HEALTH EFFECTS ACUTE HEALTH EFFECTS SWALLOWED ! Accidental ingestion of the material may be damaging to the health of the individual. ! Dusts of titanium and titanium compounds are thought to exhibit little orno toxic effects. ! Following ingestion, a single exposure to isopropyl alcohol produced lethargy and non-specific effects such as weight loss and irritation. Ingestion of near-lethal doses of isopropanol produces histopathological changes of the stomach, lungs and kidneys, incoordination, lethargy, gastrointestinal tract irritation, and inactivity or anaesthesia.