The influence of temperature on the phase behavior of ionic liquid aqueous two-phase systems

In this article, the equilibrium behavior of solutions of 1-ethyl-3-methylimidazolium dimethyl phosphate ([Emim]DMP) and ethyl acetate or acetone in aqueous two-phase system (ATPS) was discussed to understand the liquid–liquid equilibrium (LLE) behavior of these organic solvents. Thus, we determined phase diagrams and LLE data at 303.15, 308.15, 313.15, and 323.15 K for the investigated biphasic systems. Four empirical equations were used to study the tie lines. The results showed that for the [Emim]DMP?+?acetone?+?water biphasic systems within the investigated temperature range, temperature influences the phase behavior, but for the [Emim]DMP?+?ethyl acetate?+?water biphasic systems within the investigated temperature range, there are no notable changes on the phase behavior with rising temperature. The results may have important applications for the separation of antibiotics and for the recovery of ionic liquids (ILs).     

Catalytic Hydrocyanation of Activated Terminal Alkynes

A universal, practical and scalable organocatalytic hydrocyanation manifold to provide β-substituted acrylonitriles bearing an electron-withdrawing functionality has been implemented. The catalytic manifold operates under the reactivity generation principle “a good nucleophile generates a strong base”, and it uses 1,4-diazabicyclo[2.2.2]octane (DABCO) as the catalyst, activated terminal alkynes as substrates and acetone cyanohydrin as the cyanide source. The acrylonitriles obtained as E,Z mixtures are straightforwardly resolved by simple flash chromatography delivering the pure isomers in preparative amounts.     

Asymmetric cross-aldol reaction of isatin and ketones catalyzed by crude earthworm extract as efficient biocatalyst

ABSTRACT

The asymmetric cross-aldol reaction of simple ketones (acetone, cyclohexanone) with isatin derivatives in the presence of crude extract from earthworms as green and effective biocatalyst proceeds easily in MeCN/H₂O (1:1) as solvent to afford 3-hydroxy-2-oxindoles derivatives. Ten compounds were synthesized in high yields (62–88%) and moderate ee (29–42%). Structure of the synthesized compounds has been characterized on the basis of NMR spectra and CHN analysis. The ee of the obtained compounds was determined by chiral phase HPLC analysis.     

A facile one-pot three-component synthesis of benzylideneamino-3,5-dimethyl-1H-pyrazoles

A facile, one-pot three-component protocol for the synthesis of substituted 4-(benzylideneamino)-5-(3,5-dimethyl-1H-pyrazol-1-yl)-4H-1,2,4-triazole-3-thiols have been reported by the reaction of 4-amino-5-hydrazinyl-4H-1,2,4-triazole-3-thiol with acetyl acetone and various substituted benzaldehydes via multi component reaction. The newly synthesized derivatives were characterized by their elemental analysis and spectral data. The current strategy provides heterocyclic compounds in good yields with broad substrate scope.     

Structure of malagashanine,a new alkaloid with chloroquine-potentiating action

The molecular structure of malagashanine (C₂₃H₃₀N₂O₄), a new alkaloid occurring in MadagascanStrychnos species and showing chloroquine-potentiating action, has been determined by single crystal X-ray diffraction. The crystals, in the form of a 11 acetone solvate, are monoclinic, space group P2₁, witha=10.328(2),b=10.554(6),c=11.490(5)Å, =96.67(2)⁰,Z=2. Refinement based on 3650 reflections measured at 294K yieldedR=0.045. The X-ray analysis shows that the ring system in malagashanine differs from that in alkaloids of the strychnobrasiline type in containing only five-and six-membered rings. Thermal analysis of the solvate indicates that the acetone molecules are firmly held in the crystal and the X-ray analysis reveals that they are trapped in crystal voids. Only van der Waals forces and C–H...O hydrogen bonds stabilize the crystal structure.     

Bubble point measurements of binary mixtures formed by ethyl benzene with selected compounds at 95.35 kPa

Bubble point temperatures (at 95.35 kPa) over the entire composition range were measured for the binary mixtures formed by ethyl benzene with: acetyl acetone, o-, and p-cresols, 1-hexanol, and tetraethoxysilane, employing a Swietoslawski type ebulliometer. Wilson equation was used to represent the measured liquid phase composition versus bubble point temperature data, and the computed values of the vapor phase mole fractions, activity coefficients, and excess Gibbs free energy were tabulated and briefly discussed.     

Detection of acetone in the human breath as diabetes biomarker based on PPy/WO3 nanocomposite sensor by FFT continuous cyclic voltammetry method

This research represents a novel detection method of acetone level in the exhaled breath samples (RH=88 %) based on polypyrrole/tungsten oxide (PPy/WO₃) nanocomposite sensor. The PPy/WO₃ sensor was fabricated by the deposition of nanocomposite on/between interdigitated electrodes (IDEs) through electrospray coating and was then characterized by FE-SEM imaging. In this detection method, the coulometric signal of the sensor was calculated using Fast Fourier Continuous Cyclic Voltammetry (FFTCCV), where cyclic voltammetry (CV) was applied to the sensor in the defined potential rang and then charge changes of the sensor was obtained by integration of the current in all scanned potential ranges. FFTCCV method enhances the sensitivity of the sensor when exposed to the gas mixtures containing acetone. In addition to its fast coulometric response time (≤5 s) in the two linear ranges of 0.7–2.8 ppm and 2.8–28.2 ppm (R²=0.99), FFTCCV method provides the low detection limit of 70 ppb, and high sensitivity toward acetone at the optimum values of the parameters. The fabricated sensor showed great selectivity toward acetone when exposed to humid air and some exhaled gas like carbon dioxide, ammonia, methanol, ethanol and alkyl amines. The results were very satisfying as the sensor was capable to detect different acetone levels in human exhaled breath as non-invasive diagnosis of diabetes with a good correlation (R²≃0.9) to the routine blood sugar test taken by different commercial glucometers results.     

丙酮/水混合体系合成聚苯胺的聚合过程研究

对丙酮/水体系中合成聚苯胺(PAn)的反应进行跟踪,通过聚合过程的开路电压、聚合温度、特性粘度和中间体的分子结构对聚合过程进行研究。结果表明,丙酮/水体系对控制产物的粒度和分子量都有利;当丙酮/水的体积比为0.2左右时,所得产物的各项性能较好。与水体系相比,在丙酮/水混合体系中聚合过程维持高电位的时间延长,聚合链增长时间和自加速反应时间也有延长。苯胺聚合是以头-尾连接形式进行,且中间产物由高氧化态逐渐转变成中间氧化态。     

铕(Ⅲ)、铽(Ⅲ) β-二酮配合物的制备及表征

醋酸铕、醋酸铽分别与乙酰丙酮在60°C水浴下加热回流,生成两种稀土β-二酮配合物,即乙酰丙酮铕(Eu(acac)3?3H2O)和乙酰丙酮铽(Tb(acac)3?3H2O),在紫外灯下观察配合物发光现象,乙酰丙酮铕在紫外灯下显暗红色,乙酰丙酮铽在紫外灯下显亮绿色。红外分析结果与理论相吻合,荧光分析表明它们是较好的荧光材料,热分析结果说明它们的热稳定性相对较高。