Vol 10, No 3 (2019)

September 2019

Table of Contents


Hakan Arslan
DOI 10.5155/eurjchem.10.3.i-ii.1918
Editorial Board
Hakan Arslan
DOI 10.5155/eurjchem.10.3.iii-vi.1919
Graphical Contents

Research Article

Koffi Senam Etse, Guillermo Zaragoza, Bernard Pirotte
DOI 10.5155/eurjchem.10.3.189-194.1903

The hydrolysis of 2-methyl-2H-1,2,4-benzothiadiazine 1,1-dioxide (2) during crystallization under humidity (85 %) conditions, lead to N-(2-(N-methylsulfamoyl)phenyl)formamide as second step hydrolysis product, identified in the proposed degradation mechanism. Crystal of N-(2-(N-methylsulfamoyl)phenyl)formamide C8H10N2O3S (4), was obtained and characterized. The molecular structure determination was carried out with MoKα X-ray and data measured at 100 K. The compound 4 crystallizes in triclinic 1 space group with unit cell parameters a = 4.8465(4) Å, b = 8.1942(9) Å, c = 11.8686(13) Å, α = 77.080(4)°, β = 82.069(4)°, γ = 80.648(4)°, V = 450.76 (8) Å3 and Z = 2. The crystal structure is stabilized by intramolecular N-H···O and intermolecular C-H···O and N-H···O hydrogen bonds that extended as infinite 1D chain along [100]. Stabilization is also ensured by oxygen-π stacking interaction between the aromatic ring and oxygen of the sulfonamide group. The analysis of intermolecular interactions through the mapping of dnorm and shape-index revel that the most significant contributions to the Hirshfeld surface 40.6 and 33.9% are from H···H and O···H contacts, respectively.

Emmanuel Ngwang Nfor, Andrew David Burrows, Bridget Ndoye Ndosiri, Luke Lawrence Keenan, Offiong Efanga Offiong
DOI 10.5155/eurjchem.10.3.195-200.1888

A new copper(I) pyrazine-bridged coordination polymer [Cu2(pyz)3(NO3)2]·2DMF] (pyz = pyrazine) (1) has been synthesized and characterized by FT-IR, TG/DTG, DSC and single crystal X-ray diffraction techniques. The X-ray crystallographic result reveals a two-dimensional network structure containing hexagonal pores. Thermal analysis of compound 1 reveals it is stable to 380 °C, and gas sorption studies showed that it adsorbs 1.04 wt% hydrogen at 1 atm and 77 K. Compound 1 crystallizes in a triclinic system, space group P-1 (no. 2), a = 7.9550(2) Å, b = 7.9810(2) Å, c = 11.0660(3) Å, α = 76.328(1)°, β = 71.115(1)°, γ = 84.577(1)°, = 645.79(3) Å3, Z = 2, T = 150(2) K, μ(MoKα) = 1.709 mm-1, Dcalc = 1.639 g/cm3, 11111 reflections measured (7° ≤ 2Θ ≤ 54.96°), 2951 unique (Rint = 0.0539) which were used in all calculations. The final R1 was 0.0346 (>2σ(I)) and wR2 was 0.0727 (all data).

Pokpa Haba, Adama Sy, Farba Bouyagui Tamboura, Mamour Sarr, Ibrahima Elhadji Thiam, Aliou Hamady Barry, Mohamed Lamine Sall, Mohamed Gaye, Pascal Retailleau
DOI 10.5155/eurjchem.10.3.201-208.1881

Reactions of the Schiff base N,N-dimethyl-N'-((5-methyl-1H-imidazol-4-yl)methylene) ethane-1,2-diamine (HL), synthesised in situ, with chloride or thiocyanate copper (II) salt; afforded two new mononuclear complexes, [Cu(HL)Cl2]·H2O (1) and [Cu(HL)(SCN)2] (2). These compounds have been studied and characterized by elemental analysis, IR and UV-Vis spectroscopies, electrochemistry, molar conductivity and room temperature magnetic measurements. Single crystal X-ray structure determination of the complexes revealed the presence of neutral moieties in the asymmetric unit. The mononuclear (1) crystallises in the monoclinic space group P21/c with the following unit cell parameters a = 7.4355(3) Å, b = 7.2952(3) Å, c = 26.2729(11) Å, β = 93.461(4)°, V = 1422.52(10) Å3, Z = 4, R1 = 0.033 and wR2 = 0.082 and the mononuclear complex (2) crystallises in the monoclinic space group C2/c with the following unit cell parameters a = 26.2578(7) Å, b = 7.4334(2) Å, c = 16.6237(5) Å, β = 99.089(3)°, V = 3203.95(16) Å3, Z = 8, R1 = 0.037 and wR2 = 0.104. In both complexes the ligand acts in tridentate fashion and the coordination environment of the copper atom can be described as distorted square pyramidal. The crystal lattice of the complex 1 is stabilized by electrostatic forces of attraction and O–H···Cl, C–H···O, N–H···Cl, and C–H···Cl, hydrogen bonding interactions while the crystal lattice of the complex 2 is stabilized by N–H···S and C–H···N.

Mounir Abbas Ali Mohamed, Hanan Salah, Ahmed Mohamed Mohamed El-Saghier
DOI 10.5155/eurjchem.10.3.209-217.1850

Synthesis of some new bis(chalcones)-based thienothiophene derivatives and study of their synthetic utilities as building blocks for new bis(thiazole), bis(dihydropyran), bis(dihydro pyridine), bis(isoxazoles), bis(pyrazoles), bis(hydropyrimidinethiones), bis(tetrahydro diazepines, oxazepines) and bis(dihydrobenzodiazepnies, benzoxazepines) each linked to a thienothiophene core, is reported. Biological evaluation of the obtained compounds as antibacterial agents was achieved. Compounds 4b, 4c, 7a, 6a, 9a and 11b were found to be very potent against P. aeruginosa, E. coli and K. pneumonia.

Hany Hunter Monir, Adel Magdy Michael, Christine Kamal Nessim, Yasmin Mohamed Fayez, Nahla Salah Elshater
DOI 10.5155/eurjchem.10.3.218-223.1880

New, validated and accurate reversed phase HPLC method with UV detection has been established for simultaneous determination of a veterinary binary mixture of doxycycline hydrochloride (DOX) and tylosin tartrate (TYT). The stationary phase was ACE- 126-2546 AQ C-18 (250 × 4.6 mm i.d., 5 μm particle size) column at 25 °C, in an isocratic mode, using mobile phase containing a mixture of methanol: acetonitrile: distilled water in the ratio of 60:20:20 (v:v:v), with 0.01% trichloroacetic acid at the flow rate of 0.8 mL/min and UV detection was performed at 270 nm. The retention times were 4.02±0.01 and 5.62±0.01 mins for DOX and TYT, respectively. Selective determination of the cited veterinary drugs has been developed in their formulation. The method was found to be linear over 1-50 µg/mL for DOX and TYT with mean percentage recoveries 99.62±1.220 and 100.09±1.104%. The method was proven to be accurate, precise and specific. The obtained results were statistically compared with those of the official and reported methods; using Student’s t test, F test and one-way ANOVA, showing no significant difference with high accuracy. Specificity of the applied method was assessed by analysing the laboratory-prepared mixtures and their combined dosage form. The developed method was confirmed according to ICH guidelines. The validated method can be considered as alternative and basic method for the routine determination of this fixed dose combination with minimum sample preparation.

Hourieh Alkadi, Jihad Altal
DOI 10.5155/eurjchem.10.3.224-227.1840

The effect of microwave heat has been evaluated for reduction of Aflatoxin B1 and Ochratoxin A in artificially contaminated maize flour. Contaminated maize flour were heated in microwave for various times at two different power levels. The results suggest that Aflatoxin B1 and Ochratoxin A contamination can be reduced by heating samples using microwave oven. The exposure time to heat appears to have a great effect in reduction both of the toxins in maize flour samples. It is also necessary to pay attention on initial concentrations of Aflatoxin B1 or Ochratoxin A in studied maize flour samples.

Ifiok Nseobong Uwem, Basil Nse Ita
DOI 10.5155/eurjchem.10.3.228-233.1833

Starch samples from the wild species of cocoyam (Caladium bicolor (Aiton) Vent.) and three leaf yam (Dioscorea dumentorum (Kunth) Pax.) found abundantly in the south and eastern regions of Nigeria, were characterized for their physicochemical, functional and antinutrient properties. C. bicolor had higher amylose (17.68%), carbohydrate (83.57%) and ash (2.85%) than D. dumentorum. Moisture, crude lipid, protein and fibre ranged between 7.56 to 10.29%, 0.12 to 0.15%, 0.11 to 0.13%, and 2.85 to 3.39%, respectively. The starches exhibited promising functional properties with D. dumentorum having higher dispersibility (64.85%), solubility (73.99%) and oil absorption capacity (2.15 g/g). Onset (To), midpoint (Tm), and conclusion (Tc) gelatinization temperatures ranged between 63 to 79 °C. Peak, breakdown and setback viscosity were higher in D. dumentorum than C. bicolor. Moisture sorption behavior indicated increased hygroscopy with exposure time. The starches had high antinutrient levels, with D. dumentorum having higher levels of HCN and oxalates. In addition, infrared (IR) spectra of both starches were similar. Taken together, these properties suggest the suitability of these starches for non-food applications due to their high antinutrient contents.

Fares Hezam Al-Ostoot, Jigmat Stondus, Sumati Anthal, Geetha Doddenahally Venkatesh, Yasser Hussein Eissa Mohammed, Mandayam Anandalwar Sridhar, Shaukath Ara Khanum, Rajni Kant
DOI 10.5155/eurjchem.10.3.234-238.1874

Medicinal chemistry of indole analogs constitutes important therapeutic agents with anti-oxidant, anti-HIV and anti-cancer activities. Indole nucleus is frequently found in synthetic and natural products, pharmaceuticals, functional materials, agrochemicals, etc. The title compound, N-(2-(2-(4-chlorophenoxy)acetamido)phenyl)-1H-indole-2-carboxamide (5), has been synthesized in good yield by stirring the compound N-(2-aminophenyl)-2-(4-chlorophenoxy)acetamide (3) with 1H-indole-2-carboxylic acid (4), in dry dichloromethane followed by the addition of 2,6-lutidine, and o-(benzotriazol-1-yl)-N,N,N',N'-tetramethyl uraniumtetrafluoroborate in cooled condition. Compound 5 was synthesized and characterized by the conventional spectroscopic techniques (1H NMR, 13C NMR and LC-MS) and the three-dimensional structure was elucidated by using single crystal X-ray diffraction methods. It crystallizes in the monoclinic crystal system with space group P21/c. The structure was solved by direct methods and refined by full matrix least square procedure to a final R value of 0.043 for 2490 observed reflections. Three intra-molecular interactions of the type N-H···N and C-H···N were observed. The packing of molecules in the unit cell is governed by N-H···O and C-H···O intermolecular H-boned interactions which leads to the formation of infinite staking chain along [001] direction. In addition, two weak C-H···π interactions also contribute to molecular packing.

Wafaa Abdou Zaghary, Ahmed Mostafa Abdalla, Emily Tawfik Hanna, Marwa Abdel Rahman Tohamy Zanoun
DOI 10.5155/eurjchem.10.3.239-243.1786

A simple and sensitive ultra-performance liquid chromatography with Tandem Mass Spectrometric detection (UPLC-MS/MS) method was developed and validated for the simultaneous quantitation of two food colouring matters, Curcumin (CUR) and Riboflavin (RIB). Chromatographic separation was done on Hypersil gold 50×2.1 mm (1.9 μm) column, with gradient programing of mobile phase starting with aqueous 0.1% formic acid and increasing the percentage of 0.1% formic acid in acetonitrile. The utilization of multiple reaction monitoring (MRM) improved the selectivity of detection and decreased the matrix effect.  The method was linear in the range of 5-500 ng/mL for CUR and RIB. Intra- and inter-day reproducibility were within the accepted criteria. The method was successfully applied for the determination the laboratory prepared mixtures of the two selected colouring matters. The use of mass spectrometry enhanced the selectivity and sensitivity of detection which allows the robust use of the method in routine quality control tests of the two colouring matters (CUR and RIB).

Binay Prakash Akhouri, Sumit Kaur
DOI 10.5155/eurjchem.10.3.244-255.1883

In this work, we have generalized different parametric forms of cubic equations of state (EoSs) to predict complete Joule-Thomson (J-T) inversion curves for methane at wide temperature and pressure ranges. EoSs of the Soave-Redlich-Kwong (SRK), Peng-Robinson (PR), Patel-Teja (PT), Esmaeilzadeh-Roshanfekr (ER) and the Hagtalab-Kamali-Mazloumi-Mahmoodi (HKMM) along with frequently used cohesion functions α(Tr) have been considered for plot of J-T inversion curves. The PR EoS along with different cohesion functions such as those of the Soave, Antonin Chapoy and the Tau-Sim-Tassone have been also tested for accurate prediction of the inversion curves. The four parametric EoSs of Adachi-Lu-Sugie (ALS), and Lawal-Lake-Silberberg (LLS) with their associated cohesion functions have been used for the prediction of J-T inversion curves. It has been observed that for the plot of inversion curves the LLS EoS is inadequate while the ER EoS agrees well with the previous measurements made in Laboratory. Besides, the J-T coefficient measurements from EoSs have been made for carbon dioxide and nitrogen gases at temperatures from 273.15 to 473.15 K and at pressures from 10 to 1000 atm, respectively. The uncertainties of experimental J-T coefficients data of carbon dioxide from values calculated using EoSs at constant pressure of 1 atm and 20 atm and with varying temperatures have been studied.

Hong Chen, Jianchun Wu, Mingguo Liu
DOI 10.5155/eurjchem.10.3.256-262.1906

A new tetranuclear Co(II) cubane cluster 1, [Co4(L1)4(L2)4]·4CH3CH2OH (HL1 = 2-Methylquinolin-8-ol, HL2 = t-Bu-COOH), has been synthesized and characterized by X-ray single crystal diffraction, FT-IR, TG/DSC, and elementary analysis. The data reveals that it has a very interesting structural motif consisting of a [Co4O4] core in the form of a cube with the Co and O occupying opposite corners. In the crystal structure of complex 1, the molecules are linked by intramolecular CH···O hydrogen bonding interactions and Van der Waals forces, forming a three-dimensional network structure. Crystal data for complex 1: C60H68Co4N4O12, triclinic, space group P-1 (no. 2), with a = 12.0644(4), b = 12.0996(3), c = 20.2858(7) Å, α = 92.005(3)o, β = 92.182(3)°, γ = 97.943(3)°, Z = 2, V = 2928.25(16) Å3, T = 293 K, μ(Mo) = 1.178 mm-1, Dcalc = 1.444 g/cm3, 16737 reflections measured (3.00° ≤ θ ≤ 28.53°), 9010 unique (Rint = 0.024, Rsigma = 0.0574) which were used in all calculations. The final R1 was 0.039 (I≥2σ(I)) and wR2 was 0.090 (all data).

Wafaa Abdou Zaghary, Ahmed Mostafa Abdalla, Emily Tawfik Hanna, Nermeen Abdallah Shoukry
DOI 10.5155/eurjchem.10.3.263-266.1825

A coupled UPLC-MS/MS method has been developed and validated for the simultaneous quantitation of food sweeteners stevioside (STV) and aspartame (ASP). Good chromato-graphic separation was achieved on a Hypersil gold 50×2.1 mm (1.9 μm) column, using a gradient flow of 10 mM ammonium acetate, pH = 2.9 adjusted with formic acid, and 10 mM ammonium acetate in acetonitrile:water (95:5, v:v) as the mobile phase. The eluate was introduced to ESI-Mass spectrometer and scanned using multiple reaction monitoring (MRM). The method was robust, reproducible and easy to use and was validated according to ICH guidelines for the accuracy and precision giving acceptable ranges. The utilization of multiple reaction monitoring improved the selectivity of detection. Method was linear in the ranges of 2-250 ng/mL for STV and ASP. Application of this method on laboratory mixtures of the selected sweeteners was successful. The using of mass spectrometry make the method selective and measurement did not affect the presence of impurities, additive and other ingredients of detection due to the simplicity and sensitivity of this method allows the utilization of method in quality control of STV and ASP.

Bridget Ndoye Ndosiri, Katia Nchimi Nono, Paboudam Gbambie Awawou, Emmanuel Ngwang Nfor, Aminou Mohamadou, Jerome Marrot, Peter Ndifon Teke
DOI 10.5155/eurjchem.10.3.267-272.1914

The dinuclear compound, [Mn2(Pyala)2(Dca)2(H2O)]n·2H2O (1) (Pyala = N-(2-pyridylmethyl)-L-alanine and Dca = dicyanamide anion) has been synthesized and characterized by elemental analysis, IR and single crystal X-ray diffraction techniques. The crystal data for C22H26Mn2N10O6: orthorhombic, space group P212121 (no. 19), a = 10.3728(8) Å, b = 15.9780(12) Å, c = 16.3585(13) Å, = 2711.2(4) Å3, Z = 4, T = 198(2) K, μ(MoKα) = 0.989 mm-1, Dcalc = 1.559 g/cm3, 129607 reflections measured (3.564° ≤ 2Θ ≤ 60.046°), 7923 unique (Rint = 0.0324, Rsigma = 0.0155) which were used in all calculations. The final R1 was 0.0169 (I > 2σ(I)) and wR2 was 0.0458 (all data). The obtained non-centrosymmetric dinuclear Mn(II) complex contains two unique Mn(II) cations with similar octahedral coordination environment. Photoluminescent measurements on the complex in the solid state show that it displays strong photoluminescence at 442 nm.


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