Polyethylene glycol(PEG) mediated expeditious synthetic route to 1,3-oxazine derivatives

Various 1,3-oxazine derivatives were synthesized in high yields,within shorter reaction times using PEG-400 as a safer medium/ mediator.This synthetic route is exceedingly easy and avoids the use of acid/base catalysts.     

十钨钼钒锗杂多酸复合二氧化硅凝胶的制备与质子导电性

通过溶胶-凝胶法制备了掺杂十钨钼钒锗杂多酸的二氧化硅凝胶,红外光谱证明了凝胶中有Keggin[GeW10MoVO40]5-结构的阴离子存在．在室温(18℃)下,掺十钨钼钒锗酸71％的凝胶的质子电导率为1．97×10-3S·cm-1,它们是好的质子导体．     

Traceless liquid-phase synthesis of 3-alkylamino-4,5-disubstituted-1,2,4-triazoles on polyethylene glycol (PEG)

A liquid-phase route to 3-alkylamino-4,5-disubstituted-1,2,4-triazoles has been developed, which permits the incorporation of three elements of diversity. The heterocycle was constructed upon PEG6000 (soluble polymer) modified by 4-hydroxy-2-methoxybenzaldehyde, from which a traceless cleavage could be realized with TFA/CH₂Cl₂. This method provided a library of 3-alkylamino-4,5-disubstituted-1,2,4-triazoles with reasonable yields and excellent purity.     

Adsorption of polyethylene glycol (PEG) from aqueous solution onto hydrophobic zeolite

In the present study, a hydrophobic zeolite was used as an adsorbent for the adsorption of polyethylene glycol (PEG) in water solution and electroplating solution at 25 degrees C. The adsorption capacities were determined through the adsorption isotherms in a thermostated shaker. The rate of adsorption, on the other hand, was investigated in a batch adsorber under controlled process parameters such as initial PEG concentration (30, 70, 110, 150, 200, and 300 mg x dm(-3)), agitation speed (200, 800, and 1000 rpm), and adsorbent particle size (0.72, 1.44, and 2.03 mm). A batch kinetic model, according to a pseudo-second-order mechanism, has been tested to predict the rate constant of adsorption, equilibrium adsorption capacity, time of half-adsorption, and equilibrium concentration by the fitting of the experimental data. The results of the adsorption isotherm and kinetic studies show that the adsorption process can well be described with the Langmuir and Freundlich models and the pseudo-second-order equation, respectively. Comparing the values of adsorption parameters of PEG in water solution and electroplating solution, there are no significant differences. In addition, the effective diffusion coefficient of the PEG molecule in the microporous adsorbent has been estimated at about 3.20 x 10(-8) cm(2)s(-1) based on the restrictive diffusion model.     

接枝共聚法制备聚乙二醇(PEG)/聚乙烯醇(PVA)高分子固-固相变材料性能研究

用接枝共聚法将具有相变特征的聚乙二醇(PEG)接枝到具有较高熔点的聚乙烯醇(PVA)主链上,得到了系列性能稳定的PEG/PVA高分子固-固相转变材料,用DSC,WAXD和POM对其相变行为及形态结构进行了研究.结果表明,该材料呈现出可逆的固-固相转变特性;其结晶峰值温度和相变焓比纯PEG低,接枝率对相变温度和归一化相变焓影响不大;接枝率只影响结晶与熔融行为,不影响结晶结构.     

Ammonium persulphate promoted synthesis of polyethylene glycol entrapped potassium tribromide and its application in acylation and bromination of some selective organic compounds

In this study, a new method of synthesis of polyethylene glycol supported potassium tribromide (PEG KBr3) and its application in acylation and bromination reactions are reported. Ammonium persulphate oxidizes KBr to the corresponding tribromide which is entrapped by polyethylene glycol leading to stable PEG KBr3. The reagent is proved to be highly efficient for the acylation of variety of alcohols and bromination of activated aromatic substrates. Themethod is a mild, one pot reaction and involves no use of toxic reagents.     

Polyethylene glycol (PEG) promoted hydrodehalogenation of aryl halides

Transition-metal-free hydrodehalogenation of aryl halides (eg. bromides) can take place efficiently in the presence of green polyethylene glycol (PEG-800) and t-BuOK without adding any extra solvents and additives. A radical mechanism is proposed for this transition-metal-free dehalogenation of aryl halides and the role of polyethylene glycol is both reaction promotor and activated alkyl CH donor.     

Facile polyethylene glycol (PEG-400) promoted synthesis of β-ketosulfones

An efficient and convenient synthesis of β-ketosulfones is described. Reaction of an α-haloketone with sodium alkyl/aryl sulphinate yields the corresponding β-ketosulfone promoted by polyethylene glycol (PEG-400) as an efficient reaction medium.     

Size exclusion chromatography with Corona charged aerosol detector for the analysis of polyethylene glycol polymer

A technique of using size exclusion chromatography (SEC) with the Corona charged aerosol detector (CAD) was developed and evaluated in comparison with refractive index (RI) and evaporative light scattering detection (ELSD) for fast screening of polyethylene glycol (PEG), a polymer used in preparing pegylated pharmaceutical compounds. These detection techniques were used in the analysis of multiple lots of PEG reagents. CAD was found to provide more accurate impurity and polydispersity profiles of PEG reagents that better differentiate their quality, while RI was not suitable for this application due to its low sensitivity and ELSD led to underestimation of the impurity and polydispersity. The accuracy of polydispersity determination by SEC-CAD was validated against a commercial reference standard of known polydispersity. The SEC-CAD technique and the observed differences between the three detectors can also be applied to polymer analysis in general.     

PEG接枝氧化石墨烯的制备与细胞成像

通过酯化反应将不同分子量的聚乙二醇(PEG)接枝到氧化石墨烯(GO)表面,得到系列GO-PEG。利用傅里叶变换红外光谱(FTIR)、拉曼光谱(Raman)、扫描电子显微镜(SEM)对GO-PEG的结构和形貌进行了表征,用热重分析(TGA)测定了GO-PEG中PEG的接枝量。SEM结果表明GO-PEG的剥离程度高于GO。GO-PEG在磷酸盐缓冲溶液中具有良好的分散稳定性,稳定性与接枝量呈正相关。GO-PEG通过非共价键合作用对荧光素(Flu)的负载量可达1.75 mg·mg-1,且负载量受接枝量影响;另外,GO-PEG对Flu的释放行为具有pH值触发药物释放性能。将接枝PEG的端羟基与Flu共价键合,所得GO-PEG6000-Flu荧光探针实现了对HepG2细胞的成像。     

PEG接枝氧化石墨烯的制备与细胞成像

通过酯化反应将不同分子量的聚乙二醇（PEG）接枝到氧化石墨烯（GO）表面,得到系列GO-PEG。利用傅里叶变换红外光谱（FTIR）、拉曼光谱（Raman）、扫描电子显微镜（SEM）对GO-PEG的结构和形貌进行了表征,用热重分析（TGA）测定了GO-PEG中PEG的接枝量。SEM结果表明GO-PEG的剥离程度高于GO。GO-PEG在磷酸盐缓冲溶液中具有良好的分散稳定性,稳定性与接枝量呈正相关。GO-PEG通过非共价键合作用对荧光素（Flu）的负载量可达1.75mg·mg^-1,且负载量受接枝量影响;另外,GO-PEG对Flu的释放行为具有pH值触发药物释放性能。将接枝PEG的端羟基与Flu共价键合,所得GO-PEG₆₀₀₀-Flu荧光探针实现了对HepG₂细胞的成像。     

Polyethylene glycol (PEG) mediated green synthesis of 2,5-disubstituted 1,3,4-oxadiazoles catalyzed by ceric ammonium nitrate (CAN)

Abstract

Ceric ammonium nitrate in polyethylene glycol has been used as a sustainable, non-volatile, and ecofriendly catalytic medium for the green synthesis of 2,5-disubstituted 1,3,4-oxadiazoles. This protocol is effective toward various substrates having different functionalities. The easy recyclability of the reaction medium makes the reaction economically and potentially viable for commercial applications.     

AGET ATRP of methyl methacrylate with poly(ethylene glycol) (PEG) as solvent and TMEDA as both ligand and reducing agent

Activator generated by electron transfer atom transfer radical polymerization of methyl methacrylate (MMA) in inexpensive, non-toxic poly(ethylene glycol) (PEG), with air-stable Cu(II)X₂(X = Br, Cl) as the catalyst and N,N,N′,N′-tetramethylethylenediamine (TMEDA) as both ligand and reducing agent was investigated. The polymerizations in PEG proceeded in a well-controlled manner as evidenced by kinetic studies and chain extension results. The polydispersity of the polymer obtained was quite narrow, with a weight-average molecular weight/number-average molecular weight ratio of less than 1.2. Effects of the TMEDA content and the catalysts on polymerization were also investigated, respectively.     

A simple and green procedure for the conjugate addition of thiols to conjugated alkenes employing polyethylene glycol (PEG) as an efficient recyclable medium

Polyethylene glycol (PEG) is found to be an inexpensive, nontoxic, environmentally friendly reaction medium for the conjugate addition of thiols to conjugated alkenes to afford the corresponding adducts in excellent yields under mild and neutral conditions. Products of undesirable side reactions resulting from polymerization are not observed. The use of PEG avoids the use of either acid or base catalysts for this conversion and moreover PEG can be recovered and reused.     

Effect of polyethylene glycol (PEG-400) on the 1-butyl-3-methylimidazolium tetrafluoroborate-in-cyclohexane ionic liquid microemulsion

The effect of a common polymer, polyethylene glycol with molecular weight of 400 (PEG-400) on the microstructure of 1-butyl-3-methylimidazolium tetrafluoroborate (bmimBF₄)/Triton X-100/cyclohexane ionic liquid (IL) reverse microemulsion has been investigated. The addition of PEG-400 leaded to the linear increase of the microemulsion droplet size, in accordance with the observation of dispersed phase, showing that PEG-400 was only solubilized into the polar interior of the IL microemulsions. FTIR spectroscopic analysis indicated that the addition of PEG-400 decreased the electrostatic interaction between the oxygen atoms of OE units and the positive electrical charged imidazolium cation of bmimBF₄. At the same time, the oxygen atoms of PEG-400 can also interact with the imidazolium cation. These results suggested that small amounts of PEG-400 entered the palisade layers of the IL microemulsion. The conductivity of the IL reverse microemulsions was decreased owing to the dilution of conducting polar cores by the addition of insulative PEG-400, indicating that PEG-400 was only solubilized into the reverse IL microemulsion interior. The conclusion was further supported by viscosity measurement.     

Synthesis of proton conductive inorganic–organic hybrid membranes through copolymerization of dimethylethoxyvinylsilane with vinylphosphonic acid

Proton conductive inorganic–organic hybrid membranes were synthesized from dimethylethoxyvinylsilane (DMEVS), vinylphosphonic acid (VPA) and 3-glycidoxypropyltrimethoxysilane (GPTMS) through copolymerization followed by sol–gel process. The ratio of phosphorus to silicon in the copolymer almost corresponded to the charged molar ratio of VPA to DMEVS when the ratio of VPA to DMEVS was below 1/2. Self-standing, homogeneous, highly transparent membranes were synthesized from DMEVS–VPA copolymer and GPTMS via sol–gel condensation. Differential thermal analysis-thermogravimetry analyses indicated that these membranes were thermally stable up to 200 °C. The results of Fourier transform infrared and ¹³C NMR revealed that phosphonic acid groups of VPA were chemically bound to organosiloxane network. The copolymerization and condensation of (DMEVS–VPA)/GPTMS were confirmed by ³¹P and ²⁹Si NMR spectra. The proton conductivity of the hybrid membranes increased with phosphonic acid content. The membrane of (DMEVS–VPA)/GPTMS showed a remarkable conductivity of 6.3 × 10⁻² S cm⁻¹ at 130 °C and 100% relative humidity.     

pH‐Dependent Nitrotyrosine Formation in Ribonuclease A is Enhanced in the Presence of Polyethylene Glycol (PEG)

Protein nitration can occur as a result of peroxynitrite‐mediated oxidative stress. Excess production of peroxynitrite (PN) within the cellular medium can cause oxidative damage to biomolecules. The in vitro nitration of Ribonuclease A (RNase A) results in nitrotyrosine (NT) formation with a strong dependence on the pH of the medium. In order to mimic the cellular environment in this study, PN‐mediated RNase A nitration has been carried out in a crowded medium. The degree of nitration is higher at pH 7.4 (physiological pH) compared to pH 6.0 (tumor cell pH). The extent of nitration increases significantly when PN is added to RNase A in the presence of crowding agents PEG 400 and PEG 6000. PEG has been found to stabilize PN over a prolonged period, thereby increasing the degree of nitration. NT formation in RNase A also results in a significant loss in enzymatic activity.     

Sodium Chloride Molar Conductance in Different Poly(ethylene glycol)–Water Mixed Solvents

The molar conductivities of NaCl in several poly(ethylene glycol)(PEG)–water “mixed solvents” are presented as a function of the PEG content in solution. Three different PEG samples, a monodispersed one and two polydispersed ones, have been used. The comparison between the molar conductivity values in the mixed solvents and the corresponding ones in pure water shows that the only effect of PEG on the ions’ motions is an obstruction effect despite the variation of the macroscopic dielectric constant induced by PEG itself. A comparison between the molar conductivities and the corresponding mutual main diffusion coefficients shows a tight correlation between the two quantities. This correlation is possible only in the absence of electrostatic effects due to the presence of PEG.     

Solvent effects on the dielectric dispersion of poly(vinyl pyrrolidone)-poly(ethylene glycol) blends

The complex relative dielectric function , loss tangent , complex electric modulus and alternating current electrical conductivity dispersion behaviour of liquid poly(vinyl pyrrolidone)-poly(ethylene glycol) (PVP–PEG) blends in water, ethyl alcohol and 1,4–dioxane solvent over the entire volume mixture concentration range has been investigated in the frequency range of 20 Hz to 1 MHz at 25 °C. The PVP–PEG blends show the dielectric dispersion corresponding to the micro-Brownian motion of the PVP chain in the upper frequency region, whereas in the lower frequency region, dielectric dispersion is due to ionic conduction and electrode polarization phenomena. Results show that the conductivity values of these blends in water and dioxane can be monitored with the change in the solvent concentration, whereas it has a small variation with ethyl alcohol concentration. The comparative dielectric dispersion shape study confirms that the chain dynamics of polymers blend is influenced by heterogeneous interactions and solvent polar strength.     

FeBr3/Me6TREN催化MMA反向原子转移自由基聚合研究

对FeBr3/Me6TREN催化的反向原子转移自由基聚合进行了研究.在不同的催化剂、引发剂的配比、聚合温度和配体用量等条件下,该催化体系催化的MMA聚合反应动力学为一级反应,聚合物分子量可控,分子量分布很窄,说明该体系催化的聚合反应为活性可控聚合.通过实验计算了反应的活化能,并利用UV光谱对催化剂进行了研究.