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181.
Helio G. Bonacorso Marli R. Oliveira Michelle B. Costa Letícia B. Da Silva Arci D. Wastowski Nilo Zanatta Marcos A. P. Martins 《Journal of heterocyclic chemistry》2005,42(4):631-637
A convenient and general method for the regiospecific synthesis of three novel series of 1‐(2‐thenoyl)‐, 1‐(2‐furoyl)‐ and 1‐(isonicotinoyl)‐3‐alkyl(aryl)‐5‐hydroxy‐5‐trifluoromethyl‐4,5‐dihydro‐1H‐pyrazoles, in good yields (53 – 91 %), from the cyclocondensation reactions of 1,1,1‐trifluoro‐4‐alkoxy‐4‐alkyl(aryl)‐but‐3‐en‐2‐ones, where alkyl = H and Me; aryl = ‐C6H5, 4‐CH3C6H4, 4‐CH3OC6H4, 4‐FC6H4, 4‐ClC6H4, 4‐BrC6H4, 4‐NO2CgH4 with 2‐thiophenecarboxylic hydrazide, furoic hydrazide and isonicotinic acid hydrazide, respectively, is reported. Subsequently dehydration reaction of phenyl substituted 2‐pyrazolines with P2O5 furnished the corresponding 1H‐pyrazoles as mixture of regioisomers and in low yields (35 – 36 %). 相似文献
182.
do Nascimento PC Bohrer D Ramirez A Trevisan MG Tramontina J Rohlfes AL 《Talanta》2000,52(6):1047-1054
A method for the simultaneous voltammetric determination of free sulfide and volatile alkythiols (methanethiol/ethanethiol) existing as contaminant in parenteral nutrition (PN) solutions was developed. The volatile sulfides (dihydrogensulfide and alkylthiols) formed in the formulations were distilled over 45 min at 47°C in a purpose-made Conway cell. The analytes were quantified by differential pulse cathodic stripping voltametry (DPCSV) at the hanging mercury-drop electrode and determined, simultaneously as dihydrogensulfide and alkylthiols using a 60 s preconcentration time at −300 mV (versus Ag/AgCl, Cl− 3.0 mol l−1). The voltammetric signals were directly linear proportional to the sulfides concentrations in the PN solutions in the range 3–20 μmol l−1 and detection limits of about 2 μmol l−1 were calculated. Recoveries of sulfides from PN solutions in the range 90–110% were calculated using the method and nine commercial PN formulations were analyzed. Methanethiol and ethanethiol were quantified from their composite signals, and the mutual influence of the analytes on the DPCSV measurements is discussed. 相似文献
183.
Newton L Dias Filho Devaney R do Carmo Fergus Gessner André H Rosa 《Analytical sciences》2005,21(11):1309-1316
A montmorillonite from Wyoming-USA was used to prepare an organo-clay complex, named 2-thiazoline-2-thiol-hexadecyltrimethylammonium-clay (TZT-HDTA-clay), for the purpose of the selective adsorption of the heavy metals ions and possible use as a chemically modified carbon paste electrode (CMCPE). Adsorption isotherms of Hg2+, Pb2+, Cd2+, Cu2+, and Zn2+ from aqueous solutions as a function of the pH were studied at 298 K. Conditions for quantitative retention and elution were established for each metal by batch and column methods. The organo-clay complex was very selective to Hg(II) in aqueous solution in which other metals and ions were also present. The accumulation voltammetry of Hg(II) was studied at a carbon paste electrode chemically modified with this material. The mercury response was evaluated with respect to the pH, electrode composition, preconcentration time, mercury concentration, "cleaning" solution, possible interferences and other variables. A carbon paste electrode modified by TZT-HDTA-clay showed two peaks: one cathodic peak at about 0.0 V and an anodic peak at 0.25 V, scanning the potential from -0.2 to 0.8 V (0.05 M KNO3 vs. Ag/AgCl). The anodic peak at 0.25 V presents excellent selectivity for Hg(II) ions in the presence of foreign ions. The detection limit was estimated as 0.1 microg L(-1). The precision of determination was satisfactory for the respective concentration level. 相似文献
184.
Marcelo R. L. Oliveira José E. J. C. Graúdo Nivaldo L. Speziali Vito M. De Bellis 《Structural chemistry》1999,10(1):41-45
Potassium N-4-methylphenylsulfonyldithiocarbimate, K2(4-CH3C6H4SO2N=CS2), reacted with nickel(II) chloride hexahydrate and tetrabutylammonium bromide to form the bis(N-4-methylphenylsulfonyldithiocarbimate)nickelate(II) tetrabutylammonium salt (Bu4N)2[Ni(4-CH3C6H4S2C=NSO2)2]. The elemental analyses, IR and UV-Vis data obtained were consistent with the formation of a
diamagnetic planar complex. The 1H NMR and the 13C NMR spectra showed the expected signals for the dithiocarbimate moiety and the tetrabutylammonium cation. The single-crystal structure analysis showed that this substance crystallizes in the triclinic
space group with a = 10.474(3) Å, b = 10.767(3) Å, c = 13.657(3) Å and = 81.54(2)°, = 80.44(2)°, = 67.63(2)°, V = 1398.5(8) Å3, and Z = 2. The nickel atom is coordinated to four sulfur atoms. 相似文献
185.
The development of a FIA system for the determination of total choline content in several types of milk is described. The samples were submitted to hydrochloric acid digestion before injection into the system and passed through an enzymatic reactor containing choline oxidase immobilised on glass beads. This enzymatic reaction releases hydrogen peroxide which then reacts with a solution of iodide. The decrease in the concentration of iodide ion is quantified using an iodide ion selective tubular electrode based on a homogeneous crystalline membrane. Validation of the results obtained with this system was performed by comparison with results from a method described in the literature and applied to the determination of total choline in milks. The relative deviation was always < 5%. The repeatability of the method developed was assessed by calculation of the relative standard deviation (RSD) for 12 consecutive injections of one sample. The RSD obtained was < 0.6%. 相似文献
186.
187.
Joseína Moutinho Tavares de Souza Maria do Carmo Rangel 《Reaction Kinetics and Catalysis Letters》2002,77(1):29-34
The replacement of chromium by aluminium in high temperature shift catalysts was investigated. It was found that aluminium-doped hematite is a convenient candidate as an environmental friendly catalyst. 相似文献
188.
189.
190.
Muhammad Rafiq Muhammad Khalid Muhammad Nawaz Tahir Muhammad Umair Ahmad Muhammad Usman Khan Muhammad Moazzam Naseer Ataualpa Albert Carmo Braga Shabbir Muhammad Zahid Shafiq 《应用有机金属化学》2019,33(11)
Present study advocates the joint experimental and computational studies of two potent benzoimidazole‐based hydrazones with chemical formula C23H18F2N4O ( 5a ) and C25H22FN5O3 ( 5b ). Both 5a and 5b were synthesized and resolved into their crystal structures using SC‐XRD for the assessment of bond lengths, bond angles, unit cells and space groups. The structures of 5a and 5b were chemically characterized using infrared (FT‐IR), UV–Visible, nuclear magnetic resonance (1H‐NMR and 13C‐NMR), EIMS and elemental analysis. DFT at M06‐2X/6‐31G(d,p) level of theory was performed to get optimized structures and countercheck the experimental findings. Overall, DFT findings show excellent concurrence with the experimental data which confirms the purity of both compounds. FMO, NBO analysis, MEP surfaces and nonlinear optical (NLO) properties were explored at same level of theory. UV–Vis analysis at TDDFT/M06‐2X/6‐31G(d,p) level of theory showed that 5b is red shifted with λmax 331.69 nm as compared to 5a with λmax 240.25 nm. Global reactivity parameters were estimated using energy of FMOs indicated the greater harness value than the softness values of 5a and 5b . NBO analysis confirmed that the presence of non‐covalent interactions, hydrogen bonding and hyper conjugative interactions are pivotal cause for the existence of 5a and 5b in the solid‐state. NLO results of 5a and 5b were observed better than standard molecule recommended the NLO activity of said molecules for optoelectronic applications. 相似文献