A photo-oxidation of croconic acid into oxalic acid

1995 ◽  
Vol 73 (8) ◽  
pp. 1298-1304 ◽  
Author(s):  
Paul-Louis Fabre ◽  
Paule Castan ◽  
Diane Deguenon ◽  
Nicole Paillous
Keyword(s):  
Nmr Spectroscopy ◽  
Oxalic Acid ◽  
Electrochemical Oxidation ◽  
Oxidation Process ◽  
Aqueous Media ◽  
Oxidation Products ◽  
Acid Oxidation ◽  
Experimental Conditions ◽  
Photo Oxidation ◽  
C Nmr

Croconic acid, H2C5O5, is readily oxidized. This may be attested by decolorization of the solutions and by observation of oxalic acid complexes. The oxidation products are identified by 13C NMR spectroscopy as oxalic and mesoxalic acids, and experimental conditions are specified. The oxidation process requires dioxygen and photons. In parallel, the electrochemical oxidation of croconic acid is studied in aqueous media and in acetonitrile. A potential–pH diagram is drawn. Keywords: croconic acid, oxalic acid, oxidation, electrochemistry, photochemistry.

scholarly journals Elucidation and Characterization of New Chlorinated By-Products after Electrochemical Degradation of Hydrochlorothiazide Using Graphite–Poly Vinyl Chloride Electrode

Catalysts ◽  
2018 ◽  
Vol 8 (11) ◽  
pp. 540
Author(s):  
Zainab Mussa ◽  
Fouad Al-Qaim ◽  
Ali Yuzir ◽  
Hirofumi Hara ◽  
Shamila Azman ◽  
...  
Keyword(s):  
Electrochemical Oxidation ◽  
Treatment Process ◽  
Oxidation Process ◽  
Electrochemical Treatment ◽  
Electrochemical Process ◽  
Experimental Conditions ◽  
E Coli ◽  
Flight Mass Spectrometry ◽  
Negative Ionization ◽  
By Products

This paper describes an electrochemical treatment process of hydrochlorothiazide (HDZ) under different conditions such as initial concentration, sodium chloride and applied voltage. In this present study, HDZ was treated by electrochemical oxidation process using graphite-PVC composite electrode as anode and Platinum (Pt) as cathode. All results were analyzed using liquid chromatography-time of flight/mass spectrometry (LC-TOF/MS). It was found that at high applied voltages, and high amounts of NaCl, the electrochemical treatment process was more efficient. The removal% of HDZ was 92% at 5 V after 60 min. From the obtained results, the electrochemical oxidation process of HDZ followed pseudo first order with rate constant values ranged between 0.0009 and 0.0502 min−1, depending on the experimental conditions. Energy consumption was also considered in this study, it was ranged between 0.9058 and 5.56 Wh/mg using 0.5, 0.3 and 0.1 g NaCl within interval times of (10, 20, 30, 40, 50, 60, 70, and 80 min). Five chlorinated and one non-chlorinated by-products were formed and analyzed in negative ionization (NI) mode during the electrochemical process. Due to the strong oxidizing potential of the chlorine (Cl2) and hypochlorite ion (ClO−), HDZ and its by-products were removed after 140 min. Furthermore, a novel synthesis of chlorothiaizde as one of the new by-products was reported in this present study. Toxicity was impacted by the formation of the by-products, especially at 20 min. The inhibition percentage (I%) of E. coli bacteria was decreased to be the lowest value after 140 min.

Efficient removal of diuretic hydrochlorothiazide from water by electro-Fenton process using BDD anode: a kinetic and degradation pathway study

2019 ◽  
Vol 16 (8) ◽  
pp. 613 ◽  
Author(s):  
Hélène Monteil ◽  
Nihal Oturan ◽  
Yoan Péchaud ◽  
Mehmet A. Oturan
Keyword(s):  
Electrochemical Oxidation ◽  
Oxidation Reaction ◽  
Oxidation Process ◽  
Aqueous Media ◽  
Degradation Pathway ◽  
Constant Current ◽  
Gas Chromatography Mass Spectrometry ◽  
Aqueous Environment ◽  
Fenton Process ◽  
Kinetic Rate Constant

Environmental contextHydrochlorothiazide, a common diuretic pharmaceutical, occurs in environmental waters because current treatment technologies are unable to eliminate it from wastewater. To remove this environmentally hazardous chemical from water, we developed an advanced electrochemical oxidation process to efficiently degrade and mineralise the compound. Wider application of the process holds the promise of general, efficient destruction of pharmaceuticals in aqueous media. AbstractThe degradation and the mineralisation of the diuretic hydrochlorothiazide were studied by an advanced electrochemical oxidation process, ‘electro-Fenton’, which generates in situ hydroxyl radicals that are able to successfully oxidise or mineralise organic pollutants. In this study, a 0.1mM (29.8mgL−1) hydrochlorothiazide solution was completely oxidatively degraded in 15min under constant current electrolysis at 500 mA. The absolute kinetic rate constant of the oxidation reaction was also determined as (4.37±0.04)×109M−1s−1. The quasi-complete mineralisation of the solution was obtained with electrolysis for 6h under the same applied current. Several oxidation reaction intermediates were identified using gas chromatography-mass spectrometry (GC-MS). The formed carboxylic acids during the mineralisation process were also studied; oxamic, oxalic, acetic and maleic acids were identified and their concentrations were monitored throughout the electrolysis. The ions released during the treatment were also considered. Based on these data and the total organic carbon (TOC) removal results, a possible mineralisation pathway was proposed. These findings enable the conclusion that the electro-Fenton process is an efficient and environmentally-friendly method to eliminate the hazardous drug hydrochlorothiazide from an aqueous environment.

The mechanism of formation of 2,7-dimethyl-2,6-octadiene in the synthesis of 3-methylene-7-methyl-1,6-octadiene

1983 ◽  
Vol 48 (7) ◽  
pp. 1864-1866
Author(s):  
Jan Bartoň ◽  
Ivan Kmínek
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Alkali Metal ◽  
Chromatographic Analysis ◽  
Solid Phase ◽  
Reaction Pathway ◽  
Mechanism Of Formation ◽  
Gas Chromatographic Analysis ◽  
C Nmr ◽  
Visual Observations

2,7-Dimethyl-2,6-octadiene is formed in the catalytic solution for the dimerization of 2-methyl-1,3-butadiene to β-myrcene (3-methylene-7-methyl-1,6-octadiene), as revealed by mass spectrometry and 13C NMR spectroscopy. Visual observations together with the results of gas chromatographic analysis of the catalytic solution suggest that the formation of 2,7-dimethyl-2,6-octadiene is associated with the transition of the alkali metal (sodium) from the solid phase into the solution. A reaction pathway is suggested accounting for the formation of 2,7-dimethyl-2,6-octadiene in the system.

Non-cyclol (lactame) ergot alkaloids

1982 ◽  
Vol 47 (12) ◽  
pp. 3312-3317 ◽  
Author(s):  
Josef Stuchlík ◽  
Alois Krajíček ◽  
Ladislav Cvak ◽  
Jiří Spáčil ◽  
Petr Sedmera ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Ergot Alkaloids ◽  
C Nmr

Two new alkaloids were isolated from the field ergot. Their structures, N-(D-lysergyl-L-valyl)cyclo(L-valyl-D-prolyl) (IV) and N-(D-lysergyl-L-valyl)cyclo(L-leucyl-D-prolyl) (V), were assigned by mass, 1H and 13C NMR spectroscopy.

Determination of alcohols in mixtures by 19F NMR spectroscopy using hexefluoroacetone reagent

1982 ◽  
Vol 47 (7) ◽  
pp. 1973-1978 ◽  
Author(s):  
Jiří Karhan ◽  
Zbyněk Ksandr ◽  
Jiřina Vlková ◽  
Věra Špatná
Keyword(s):  
Standard Deviation ◽  
Nmr Spectroscopy ◽  
Standard Method ◽  
Internal Standard ◽  
Internal Standard Method ◽  
Concentration Region ◽  
Experimental Conditions ◽  
Curve Method ◽  
Sample Preparation Procedure

The determination of alcohols by 19F NMR spectroscopy making use of their reaction with hexafluoroacetone giving rise to hemiacetals was studied on butanols. The calibration curve method and the internal standard method were used and the results were mutually compared. The effects of some experimental conditions, viz. the sample preparation procedure, concentration, spectrometer setting, and electronic integration, were investigated; the conditions, particularly the concentrations, proved to have a statistically significant effect on the results of determination. For the internal standard method, the standard deviation was 0.061 in the concentration region 0.032-0.74 mol l-1. The method was applied to a determination of alcohols in the distillation residue from an oxo synthesis.

An unusual reaction of a bridged triterpenoid α-diketone with acetic anhydride

1991 ◽  
Vol 56 (12) ◽  
pp. 2917-2935 ◽  
Author(s):  
Eva Klinotová ◽  
Václav Křeček ◽  
Jiří Klinot ◽  
Miloš Buděšínský ◽  
Jaroslav Podlaha ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Nmr Spectroscopy ◽  
Acetic Anhydride ◽  
Spectral Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mild Conditions ◽  
Condensation Products ◽  
Unsaturated Lactones ◽  
C Nmr

3β-Acetoxy-21,22-dioxo-18α,19βH-ursan-28,20β-olide (IIIa) reacts with acetic anhydride in pyridine under very mild conditions affording β-lactone IVa and γ-lactones Va and VIIa as condensation products. On reaction with pyridine, lactones Va and VIIa undergo elimination of acetic acid to give unsaturated lactones VIIIa and IXa, respectively. Similarly, the condensation of 20β,28-epoxy-21,22-dioxo-18α,19βH-ursan-3β-yl acetate (IIIb) with acetic anhydride leads to β-lactone IVb and γ-lactone Vb; the latter on heating with pyridine affords unsaturated lactone VIIIb and 21-methylene-22-ketone Xb. The structure of the obtained compounds was derived using spectral methods, particularly 1H and 13C NMR spectroscopy; structure of lactone IVa was confirmed by X-ray diffraction.

A New Dimeric Derivative of Ethoxyquin from Its Reaction with Alkylperoxy Radicals

1993 ◽  
Vol 58 (8) ◽  
pp. 1914-1918 ◽  
Author(s):  
Jaroslav Kříž ◽  
Luděk Taimr
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Peroxy Radicals ◽  
Methyl Group ◽  
Alkylperoxy Radicals ◽  
C Nmr

The structure of a new compound formed in the reaction of ethoxyquin with alkylperoxy radicals was resolved by 1H and 13C NMR spectroscopy (including COSY, NOESY, HHC RCT and SSLR INEPT techniques) and confirmed by mass spectrometry. The structure suggest participation of 4-methyl group of ethoxyquin in the deactivation of peroxy radicals. A mechanism of this reaction is proposed.

Reactivity of Sodium Hexaethyl-2,4-dicarba-nido-hexaborate(1-)

1999 ◽  
Vol 64 (6) ◽  
pp. 977-985 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Hans-Jörg Schanz ◽  
Wolfgang Milius ◽  
Catherine McCammon
Keyword(s):  
Mössbauer Spectroscopy ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Hydrogen Atom ◽  
Mossbauer Spectroscopy ◽  
Sandwich Complex ◽  
X Ray ◽  
Bromo Derivative ◽  
Boron Tribromide ◽  
C Nmr

Sodium hexaethyl-2,4-dicarba-nido-hexaborate(1-) (6), available from hexaethyl-2,4-dicarba- nido-hexaborane(8) (4) by deprotonation, reacts with deuterated methanol, CD3OD, to give back 4 without H/D exchange of the B-H-B hydrogen atom. The reaction of 6 with diethylboron chloride, Et2BCl, affords hexaethyl-2,4-dicarba-closo-hexaborane(6) (7), the first example of a peralkylated carborane of this type. In contrast, the reaction of 6 with boron tribromide, BBr3, leads mainly to 2,3,4,5,6,7-hexaethyl-2,4-dicarba-closo-heptaborane(7) (8), together with the corresponding 1-bromo derivative (9) and the closo-carborane 7 as side products. The reaction of two equivalents of 6 with FeCl2 gives the air-stable sandwich complex bis[hexaethyl-2,4-dicarba-nido-hexaborate(1-)]iron 10 which was characterised by X-ray structural analysis. All products were characterised by 1H, 11B and 13C NMR spectroscopy, and 57Fe Mössbauer spectroscopy was used to study 10.

Sign in / Sign up

Export Citation Format

Share Document