Thiourea Derivatives,Simple in Structure but Efficient Enzyme Inhibitors and Mercury Sensors

In this study six unsymmetrical thiourea derivatives, 1-isobutyl-3-cyclohexylthiourea (1), 1-tert-butyl-3-cyclohexylthiourea (2), 1-(3-chlorophenyl)-3-cyclohexylthiourea (3), 1-(1,1-dibutyl)-3-phenylthiourea (4), 1-(2-chlorophenyl)-3-phenylthiourea (5) and 1-(4-chlorophenyl)-3-phenylthiourea (6) were obtained in the laboratory under aerobic conditions. Compounds 3 and 4 are crystalline and their structure was determined for their single crystal. Compounds 3 is monoclinic system with space group P2₁/n while compound 4 is trigonal, space group R³:H. Compounds (1–6) were tested for their anti-cholinesterase activity against acetylcholinesterase and butyrylcholinesterase (hereafter abbreviated as, AChE and BChE, respectively). Potentials (all compounds) as sensing probes for determination of deadly toxic metal (mercury) using spectrofluorimetric technique were also investigated. Compound 3 exhibited better enzyme inhibition IC₅₀ values of 50, and 60 µg/mL against AChE and BChE with docking score of −10.01, and −8.04 kJ/mol, respectively. The compound also showed moderate sensitivity during fluorescence studies.     

The synthesis of facial amphiphile 3α,7α-diaminocholestane

The facial amphiphile 3α,7α-diaminocholestane 3 was synthesized from 3β-acetoxy-7-ketocholestane 1 through a stepwise reductive amination. The reductive amination of 1 with NH₄OAc in the presence of NaBH₃CN, and protection with Boc₂O yielded 7α-(tert-butyloxycarbonyl)-aminocholestane 4 in 86% yield. The reductive amination of 6, which was obtained from 4 after hydrolysis and subsequent oxidation, with NH₄OT_f in the presence of NaBH(OEh)₃ provided 3 in 75% yield after protection with Boc₂O.     

Synthesis and Single Crystal X-ray Studies of 3-(3,5-Bis(trifluoromethyl)phenyl) Quinoline and 3-(4-Fluoro-3-methylphenyl) Quinoline

The title compounds 3-(3,5-bis(trifluoromethyl)phenyl)quinoline(1) and 3-(4-fluoro-3-methylphenyl)quinoline(2) were synthesized through Suzuki-Miyaura Cross coupling reaction of 3-bromoquinoloine with aryl boronic acids.The title compounds were characterized by single-crystal X-ray diffraction,1H NMR,13C NMR,EI-MS,elemental analysis and IR.The crystals of 3-(3,5-bis(trifluoromethyl)phenyl)quinoline(C17H9F6N,Mr = 341.25) belongs to the monoclinic system,space group P21n,a = 12.3072(13),b = 4.9378(6),c = 24.493(2) ,V = 1473.1(3) 3,Z = 4,Dc = 1.539 Mg m-3,λ = 0.71073 ,μ = 0.144 mm-1,F(000) = 688,the final R = 0.0715 and wR = 0.1873 for 1875 observed reflections with I 2σ(I) and the crystal of 3-(4-fluoro-3-methylphenyl)quinoline(C16H12FN,Mr = 237.27) belongs to the orthorhombic system,space group Pca21,a = 23.794(2),b = 3.9094(3),c = 25.669(2) ,V = 2387.7(4) 3,Z = 8,Dc = 1.320 Mg m-3,λ = 0.71073 ,μ = 0.088 mm-1,F(000) = 992,the final R = 0.0534 and wR = 0.1188 for 2270 observed reflections with I 2σ(I).     

Two-step laser excitation of the highly excited even-parity states of atomic mercury

We report term energies and quantum defects of highly excited even-parity states of mercury in the 83 876–84 140 cm^-1 energy range, employing a two-step laser excitation scheme via the S₀↦6s6p³P₁ inter-combination transition. Two dye lasers, pumped by a common Nd:YAG laser, were frequency doubled by BBO crystals and used to record the spectra in conjunction with a thermionic diode ion detector. Our new observations include the much extended D₂ (22 ≤n ≤52) series and a few members of the S₁ (24 ≤n ≤30) Rydberg series. Members of the D₂ Rydberg series with such a high n value are reported for the first time. The relative intensities of the D₂ and S₁ transitions (m = 4, 5 and 6) of group II-B elements excited from the P₁ inter-combination states are also discussed.     

First report on the kinetics of the uncatalyzed esterification of cellulose under homogeneous reaction conditions: a rationale for the effect of carboxylic acid anhydride chain-length on the degree of biopolymer substitution

The kinetics of the homogeneous acylation of microcrystalline cellulose, MCC, with carboxylic acid anhydrides with different acyl chain-length (Nc; ethanoic to hexanoic) in LiCl/N,N-dimethylacetamide have been studied by conductivity measurements from 65 to 85 °C. We have employed cyclohexylmethanol, CHM, and trans-1,2-cyclohexanediol, CHD, as model compounds for the hydroxyl groups of the anhydroglucose unit of cellulose. The ratios of rate constants of acylation of primary (CHM; Prim-OH) and secondary (CHD; Sec-OH) groups have been employed, after correction, in order to split the overall rate constants of the reaction of MCC into contributions from the discrete OH groups. For the model compounds, we have found that k_(Prim-OH)/k_(Sec-OH) > 1, akin to reactions of cellulose under heterogeneous conditions; this ratio increases as a function of increasing Nc. The overall, and partial rate constants of the acylation of MCC decrease from ethanoic- to butanoic-anhydride and then increase for pentanoic- and hexanoic anhydride, due to subtle changes in- and compensations of the enthalpy and entropy of activation.     

Gold-surface binding of molecular switches studied by M?ssbauer spectroscopy

The nonanuclear coordination compound [Mo^IV{(CN)Fe^III(3-methyl-saldptn)}₈]Cl₄ exhibits multiple spin transitions (3-methyl-saldptn = N,N′-bis(3′′-methyl-2′′-hydroxy-benzyliden)-1,7-diamino-4-azaheptane). This spin crossover cluster is bound via a self-assembled monolayer onto a two dimensional array gold surface. M?ssbauer spectroscopy indicates that the thermally and optically induced spin crossover of the compound is maintained. Thereby, the foundation for its potential practical application (e.g. in the field of information storage) was laid.     

Vibrations of FGM thin cylindrical shells with exponential volume fraction law

In this paper, the influence of an exponential volume fraction law on the vibration frequencies of thin functionally graded cylindrical shells is studied. Material properties in the shell thickness direction are graded in accordance with the exponential law. Expressions for the strain-displacement and curvature-displacement relationships are taken from Love＇s thin shell theory. The Rayleigh-Ritz approach is used to derive the shell eigenfrequency equation. Axial modal dependence is assumed in the characteristic beam functions. Natural frequencies of the shells are observed to be dependent on the constituent volume fractions. The results are compared with those available in the literature for the validity of the present methodology.     

Vibration characteristics of FGM circular cylindrical shells filled with fluid using wave propagation approach

The vibration characteristics of a functionally graded material circular cylindrical shell filled with fluid are examined with a wave propagation approach. The shell is filled with an incompressible non-viscous fluid. Axial modal dependence is approximated by exponential functions. A theoretical study of shell vibration frequencies is analyzed for simply supported-simply supported, clamped-simply supported, and clamped-clamped boundary conditions with the fluid effect. The validity and the accuracy of the present method are confirmed by comparing the present results with those available in the literature. Good agreement is observed between the two sets of results.     

The development and validation of a solid phase extraction/HPLC method for the determination of aflatoxins in groundnut meal

Summary The efficiency of an analytical method for the determination of aflatoxins in groundnut meal has been statistically examined. The procedure consists of a phenyl bonded phase (PH) clean-up of an acetone: water (8515) extract followed by HPLC quantification. Average recoveries from spiked groundnut meal extracts were calculated to be 101.3% and 101.8%, with limits of detection of 7.4 and 2.62 g/kg for aflatoxins-B1 and-B2 respectively. Higher recoveries of aflatoxin-B1 from naturally contaminated samples were recorded using the proposed procedure than those recorded using the official AOAC (CB) method although the precisions of the two methods were not found to differ at the 5% significance level. Similar recoveries of aflatoxin-B2 were recorded for both methods but the proposed procedure was found to be more precise. The proposed PH-HPLC method was far less time consuming and more economical on solvents than the CB procedure.