Adducts of sila-, germa-, and stannaethenes Me2E=C(SiMe3)2 (E = Si, Ge, Sn) with anthracene: syntheses, structures, thermolyses

2000 ◽  
Vol 78 (11) ◽  
pp. 1412-1420 ◽  
Author(s):  
Nils Wiberg ◽  
Susanne Wagner ◽  
Sham-Kumar Vasisht ◽  
Kurt Polborn

The [4 + 2] cycloadducts of Me2E=C(SiMe3)2 (E = Si, Ge, Sn) and anthracene are prepared by reaction of an excess of anthracene in benzene with the [2 + 2] cycloadduct of Me2Si=C(SiMe3)2 and Ph2C=NSiMe3 at 130°C, with Me2Ge(OPh)-CLi(SiMe3)2 at 100°C, and with Me2SnBr-CNa(SiMe3)2 at 80°C, respectively. The mentioned adducts act as sources for the ethenes Me2E=C(SiMe3)2 above 100°C, the intermediate formation of which has been demonstrated by trapping experiments with 2,3-dimethylbutadiene (formation of a [4 + 2] and an ene reaction product). The half life time of the anthracene adducts with E = Si, Ge, and Sn in the presence of DMB (= 2,3-dimethylbutadiene) in benzene on thermolysis at 130°C (first order reactions) is found to be 141, 12, and 0.3 h, respectively. In the absence of DMB, thermolysis of the cycloadducts leads in benzene as reaction medium exclusively to the dimers of the Me2E=C(SiMe3)2 intermediates. In toluene as reaction medium ene products of Me2E=C(SiMe3)2 are observed in addition to the dimers. The ene products are not isolable as such, but only after migration of the Me2E-CH(SiMe3)2 substituents. The formed derivatives C6H5CH2EMe2CH(SiMe3)2 of toluene in part give a second ene reaction with another Me2E=C(SiMe3)2 molecule. X-ray structure analyses of the mentioned sources in fact prove the latter to be normal [4 + 2] cycloadducts of Me2E=C(SiMe3)2 and anthracene.Key words: silaethene, germaethene, stannaethene, [4 + 2] anthracene adducts, [4 + 2] cycloadditions and reversions, ene reactions, X-ray structure analyses.

1967 ◽  
Vol 20 (11) ◽  
pp. 2305 ◽  
Author(s):  
RD Brown ◽  
GP Pez

The preparation of difluorodisulphane, FSSF, by the silver fluoride/sulphur reaction is described. Difluorodisulphane is unstable at room temperature and rearranges spontaneously into thio-thionyl fluoride, SSF2. The largest observed first-order half-life time of FSSP gas was 4.7 hr at 21.8 � 0.3�. The decomposition of FSSF is catalysed by hydrogen fluoride and boron trifluoride. Chemical reactions of the isomers with AgF2, Cl2, BCl3, S2Cl2, acetone, benzoic acid, Pyrex, and quartz were studied. The absorption spectra of gaseous FSSF and SSF2 were recorded in the range of 10000 to 53000 cm-1. Medium to high intensity continua were noted with maxima for FSSF at 50200�250 and 41400�250 cm-1 and for SSF2 at 53000�500, 41400�250, and 33800�400 cm-1.


2011 ◽  
Vol 76 (8) ◽  
pp. 1093-1101 ◽  
Author(s):  
Xin-Huai Zhao ◽  
Peng Wu ◽  
Ying-Hua Zhang

Six sulfonamides, i.e., sulfadiazine, sulfadimethoxine, sulfamerazine, sulfamethazine, sulfamethoxazole and sulfamonomethoxine, were applied to spike whole hen eggs at 0.1 mg kg- 1 eggs. The spiked hen eggs were heated at 80 and 100 ?C to investigate the degradation kinetics of the sulfonamides under simulated cooking conditions. The sulfonamides added were extracted twice from the spiked eggs with dichloromethane by an ultrasonic-assistant extraction, and analyzed by a HPLC method after purification. The first-order rate constants and half-life times of the sulfonamides were calculated, and the corresponding apparent activation energy of their degradation was also obtained by application of the Arrhenius equation. The results indicated that all six sulfonamides degraded faster at the higher heating temperature, with first-order rate constants ranging from 0.0056 to 0.0108 min-1 at 80 ?C and from 0.0147 to 0.0394 min-1 at 100 ?C. The apparent activation energies for the degradation of the sulfonamides were estimated to be in the range 30.9 to 77.5 kJ mol-1. Sulfadiazine and sulfadimethoxine had the shortest and longest half-life time, respectively, and were the most instable and stable.


1983 ◽  
Vol 49 (02) ◽  
pp. 109-115 ◽  
Author(s):  
M Hoylaerts ◽  
E Holmer ◽  
M de Mol ◽  
D Collen

SummaryTwo high affinity heparin fragments (A/r 4,300 and M, 3,200) were covalently coupled to antithrombin III (J. Biol. Chem. 1982; 257: 3401-3408) with an apparent 1:1 stoichiometry and a 30-35% yield.The purified covalent complexes inhibited factor Xa with second order rate constants very similar to those obtained for antithrombin III saturated with these heparin fragments and to that obtained for the covalent complex between antithrombin III and native high affinity heparin.The disappearance rates from plasma in rabbits of both low molecular weight heparin fragments and their complexes could adequately be represented by two-compartment mammillary models. The plasma half-life (t'/j) of both low Afr-heparin fragments was approximately 2.4 hr. Covalent coupling of the fragments to antithrombin III increased this half-life about 3.5 fold (t1/2 ≃ 7.7 hr), approaching that of free antithrombin III (t1/2 ≃ 11 ± 0.4 hr) and resulting in a 30fold longer life time of factor Xa inhibitory activity in plasma as compared to that of free intact heparin (t1/2 ≃ 0.25 ± 0.04 hr).


2020 ◽  
Vol 27 ◽  
Author(s):  
Shwethashree Malla ◽  
Sathyanarayana N. Gummadi

Background: Physical parameters like pH and temperature play a major role in the design of an industrial enzymatic process. Enzyme stability and activity are greatly influenced by these parameters; hence optimization and control of these parameters becomes a key point in determining the economic feasibility of the process. Objective: This study was taken up with the objective to optimize physical parameters for maximum stability and activity of xylose reductase from D. nepalensis NCYC 3413 through separate and simultaneous optimization studies and comparison thereof. Method: Effects of pH and temperature on the activity and stability of xylose reductase from Debaryomyces nepalensis NCYC 3413 were investigated by enzyme assays and independent variables were optimised using surface response methodology. Enzyme activity and stability were optimised separately and concurrently to decipher the appropriate conditions. Results: Optimized conditions of pH and temperature for xylose reductase activity were determined to be 7.1 and 27 ℃ respectively, with predicted responses of specific activity (72.3 U/mg) and half-life time (566 min). The experimental values (specific activity 50.2 U/mg, half-life time 818 min) were on par with predicted values indicating the significance of the model. Conclusion: Simultaneous optimization of xylose reductase activity and stability using statistical methods is effective as compared to optimisation of the parameters separately.


2020 ◽  
Vol 16 ◽  
Author(s):  
M. Alarjah

Background: Prodrugs principle is widely used to improve the pharmacological and pharmacokinetic properties of some active drugs. Much effort was made to develop metronidazole prodrugs to enhance antibacterial activity and or to improve pharmacokinetic properties of the molecule or to lower the adverse effects of metronidazole. Objective: In this work, the pharmacokinetic properties of some of monoterpenes and eugenol pro metronidazole molecules that were developed earlier were evaluated in-vitro. The kinetic hydrolysis rate constants and half-life time estimation of the new metronidazole derivatives were calculated using the validated RP-HPLC method. Method: Chromatographic analysis was done using Zorbbax Eclipse eXtra Dense Bonding (XDB)-C18 column of dimensions (250 mm, 4.6 mm, 5 μm), at ambient column temperature. The mobile phase was a mixture of sodium dihydrogen phosphate buffer of pH 4.5 and methanol in gradient elution, at 1ml/min flow rate. The method was fully validated according to the International Council for Harmonization (ICH) guidelines. The hydrolysis process carried out in an acidic buffer pH 1.2 and in an alkaline buffer pH 7.4 in a thermostatic bath at 37ºC. Results: The results followed pseudo-first-order kinetics. All metronidazole prodrugs were stable in the acidic pH, while they were hydrolysed in the alkaline buffer within a few hours (6-8 hr). The rate constant and half-life values were calculated, and their values were found to be 0.082- 0.117 hr-1 and 5.9- 8.5 hr., respectively. Conclusion: The developed method was accurate, sensitive, and selective for the prodrugs. For most of the prodrugs, the hydrolysis followed pseudo-first-order kinetics; the method might be utilised to conduct an in-vivo study for the metronidazole derivatives with monoterpenes and eugenol.


1982 ◽  
Vol 47 (4) ◽  
pp. 1069-1077 ◽  
Author(s):  
Karel Mádlo ◽  
František Hanousek ◽  
Antonín Petřina ◽  
Jaroslav Tláskal

Ferrous sulphate was oxidized by potassium chlorate in the pH region 2-7 and at temperatures ranging from 298.1 to 323.1 K and various hydrolytic products of Fe(III) were separated and indentified. The separated solid ferric products were analyzed using a combination of the chemical analysis, IR spectroscopy, X-ray diffraction, and electron microscopy. The following substances were found as major components of the products: Fe2O3.n H2O ("ferric gel"), Fe2O3.n H2O with bound SO2-4 ions ("sulphogel"), α-FeO(OH), γ-FeO(OH) and Fe3O4. Their amount depends particularly on the pH temperature of the reaction medium.


1997 ◽  
Vol 62 (6) ◽  
pp. 855-865 ◽  
Author(s):  
Katarína Erentová ◽  
Vladimír Adamčík ◽  
Andrej Staško ◽  
Oskar Nuyken ◽  
Arming Lang ◽  
...  

The cathodically and photochemically induced decomposition of thioazo compounds XC6H4-N2-S-C6H4CH3 and their polymers with X = NO2, COOH, and SO3H were investigated. The formation of carbon-centered XC6H4. and sulfur-centered .S-C6H4Y radicals was confirmed using spin-trap technique. These reactive radicals either abstract hydrogen from CH3CN solvent molecule forming .CH2CN radical or they recombine to cage products XC6H4-S-C6H4CH3 eliminating N2. The decomposition rate of the investigated thioazo compounds is characterized by a formal half-life time of 5 to 10 s.


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Mohamed S. Yahia ◽  
Ahmed S. Elzaref ◽  
Magdy B. Awad ◽  
Ahmed M. Tony ◽  
Ahmed S. Elfeky

Abstract Commercial Granulated Active Carbon (GAC) has been modified using 10 Gy dose Gamma irradiation (GAC10 Gy) for increasing its ability of air purification. Both, the raw and treated samples were applied for removing Chlorpyrifos pesticide (CPF) from ambient midair. Physicochemical properties of the two materials were characterized by Fourier Transform Infrared (FT-IR) and Raman spectroscopy. The phase formation and microstructure were monitored using X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), supported with Energy-Dispersive X-ray (EDX). The Surface area measurement was detected using BET particle size prosometry. Obtained outcomes showed that, the maximum adsorption capacity, given by Langmuir equations, was greatly increased from 172.712 to 272.480 mg/g for GAC and GAC10 Gy, respectively, with high selectivity. The overall removal efficiency of GAC10 Gy was notably comparable to that of the original GAC-sorbent. The present study indicated that, gamma irradiation could be a promising technique for treating GAC and turned it more active in eliminating the pesticides pollutants from surrounding air. The data of equilibrium has been analyzed by Langmuir and Freundlich models, that were considerably better suited for the investigated materials than other models. The process kinetics of CPF adsorbed onto both tested carbon versions were found to obey the pseudo first order at all concentrations with an exception at 70 mg/l using GAC, where, the spontaneous exothermic adsorption of Chlorpyrifos is a strong function for the pseudo-first order (PFO) and pseudo second order (PSO) kinetics.


1985 ◽  
Vol 40 (11) ◽  
pp. 1128-1132
Author(s):  
Y. Riad ◽  
Adel N. Asaad ◽  
G.-A. S. Gohar ◽  
A. A. Abdallah

Sodium hydroxide reacts with α -(4-nitrobenzylthio)-acetic acid in aqueous-dioxane media to give 4,4'-diformylazoxybenzene as the main product besides 4,4'-dicarboxyazoxybenzene and a nitrone acid. This reaction was kinetically studied in presence of excess of alkali in different dioxane-water media at different temperatures. It started by a fast reversible a-proton abstraction step followed by two consecutive irreversible first-order steps forming two intermediates (α -hydroxy, 4-nitrosobenzylthio)-acetic acid and 4-nitrosobenzaldehyde. The latter underwent a Cannizzaro's reaction, the products of which changed in the reaction medium into 4,4'-diformylazoxybenzene and 4,4'-dicarboxyazoxybenzene. The rate constants and the thermodynamic parameters of the two consecutive steps were calculated and discussed. A mechanism was put forward for the formation of the nitrone acid.Other six 4-nitrobenzyl, aryl sulphides were qualitatively studied and they gave mainly 4,4'-diformylazoxybenzene beside 4,4'-dicarboxyazoxybenzene or its corresponding azo acid.


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