Synthesis of 5-alkylated barbituric acids and 3-alkylated indoles via microwave-assisted three-component reactions in solvent-free conditions using Hantzsch 1,4-dihydropyridines as reducing agents

Reaction of barbituric acids with aldehydes and dihydropyridines in one pot under microwave (MW) irradiation in the absence of solvent, affords 55–82% of the 5-benzylated barbituric acids. Use of alkyl nitriles or barbituric acids with indole-3-aldehyde and dihydropyridine (DHP) afforded 3-alkylated indoles in 57–76 % yield. In each case DHPs are converted to pyridines.     

Facile and efficient synthesis of functionalized iminothiopyran and isothiochromen via one-pot multicomponent reactions

An efficient synthesis of 6H-6-iminothiopyran-2,3-dicarboxylate and 1H-isothiochromene-3,4-dicarboxylate derivatives via one-pot reactions between acetylenic esters, aryl isothiocyanates and enaminones in dichloromethane at room temperature is described. The mild reaction condition, high yields and the new products are advantages of our method.     

Facile and rapid one-pot microwave-assisted synthesis of Pd-Ni magnetic nanoalloys confined in mesoporous carbons

An easy and rapid one-pot microwave-assisted soft-template synthesis method for the preparation of Pd-Ni nanoalloys confined in mesoporous carbon is reported. This approach allows the formation of mesoporous carbon and the growth of the particles at the same time, under short microwave irradiation (4 h) compared to the several days spent for the classical approach. In addition, the synthesis steps are diminished and no thermopolymerization step or reduction treatment being required. The influence of the Pd-Ni composition on the particle size and on the carbon characteristics was investigated. Pd-Ni solid solutions in the whole composition range could be obtained, and the metallic composition proved to have an important effect on the nanoparticle size but low influence on carbon textural properties. Small and uniformly distributed nanoparticles were confined in mesoporous carbon with uniform pore size distribution, and dependence between the nanoparticle size and the nanoalloy composition was observed, i.e., increase of the particle size with increasing the Ni content (from 5 to 14 nm). The magnetic properties of the materials showed a strong nanoparticle size and/or composition effect. The blocking temperature of Pd-Ni nanoalloys increases with the increase of Ni amount and therefore of particle size. The magnetization values are smaller than the bulk counterpart particularly for the Ni-rich compositions due to the formed graphitic shells surrounding the particles inducing a dead magnetic layer.

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Graphical abstract PdNi nanoalloys confined in mesoporous carbon exhibiting magnetic properties dependent on thealloys composition and size were synthesized by a fast microwave approach

     

Synthesis of novel 4H-pyrimido[1,6-a]pyrimidines via a one-pot three-component condensation

Abstract  

Highly substituted novel 4H-pyrimido[1,6-a] pyrimidines were prepared by a trifluoromethanesulfonic acid catalyzed one-pot three-component condensation of 4-aminopyrimidines, aldehydes, and β-ketoesters. A preliminary feasibility study was undertaken on these compounds, to assess the potential production of a library of further diversified compounds by nucleophilic replacement of Cl (R¹) or by reaction of electrophiles with the NH₂ (R²) group.     

机械合金化合成CoSb3过程中的固相反应机理的热力学解释

用Co和Sb作为初始原料,通过机械合金化(mechanical alloying,MA)的方法合成了CoSb3,并系统研究了MA转速和MA时间对MA过程中固相反应的影响.XRD结果表明,相同MA转速下,CoSb3的量随MA时间的延长而增多,但是MA时间过长会导致大量CoSb2的生成,甚至诱发CoSb3分解为CoSb2和非晶态Sb.而提高MA转速,只能缩短固相反应的发生时间,而不会改变整个固相反应趋势.对于特定的状态所对应的MA转速和MA时间满足ω3.8t=C(常数)关系,这种MA转速和MA时间的等效性,说明MA过程中能量的积累.并从非平衡热力学的角度,解释了MA过程的固相反应机理.     

Facile synthesis and capacitive performance of the Co(OH)2 nanostructure via a ball-milling method

Co(OH)₂ nanoparticles were synthesized using only CoSO₄·7H₂O and NaOH as reactants without other auxiliary reagents via a simple, low-cost and practical ball-milling technique and investigated as the active electrode materials for supercapacitors. The structure and morphology of the resulting Co(OH)₂ samples were examined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and transmission electron microscopy (TEM). The observations revealed the formation of brucite-like phase of β-Co(OH)₂, which had an irregular sphere-like shape with an average size of 50-100 nm. When investigated as electrode materials for supercapacitors, the β-Co(OH)₂ exhibited good energy-storage performances in terms of high specific capacitance of 599 F g⁻¹ and excellent capacity retention, suggesting its potential application in the electrode material for supercapacitors.     

Sonochemical synthesis of two nanostructured silver(I) coordination polymers based on semi-rigid bis(benzimidazole) ligands

Nanoparticles of two silver(I) coordination polymers (CPs), [Ag₂(L1)₂(DCTP)]_n (1) and [Ag₂(L2)(DCTP)]_n (2) (L1 = 1,3-bis(5,6-dimethylbenzimidazol-1-ylmethyl)benzene, L2 = 1,4-bis(benzimidazol-1-yl)-2-butene, H₂DCTP = 2,5-dichloroterephthalic acid), were synthesized by the sonochemical approach and hydrothermal method. Both CPs were characterized by elemental analysis, IR spectra, single-crystal X-ray diffraction, scanning electron microscopy (SEM), and thermogravimetric analyses (TGA). CP 1 exhibits a 2D 4-connected sql net with the point symbol {4⁴.6²}. While CP 2 displays a 2D 3,4-connected 3,4L13 net with the point symbol {4.6²}₂{4².6².8²}. The structural diversity indicates that semi-rigid bis(benzimidazole) co-ligands play important roles in tuning the structures of the mixed Ag(I) CPs. The ultrasound irradiation time, temperature, and power showed significant effects on the morphology and growth process of the nanoparticles of two silver(I) CPs. The luminescence and photocatalytic properties of the nanoparticles of CPs 1–2 on the degradation of methyl blue (MB) were also investigated in detail.     

A novel method for the synthesis of substituted 3,4-dihydrocoumarin derivatives via isocyanide-based three-component reaction

A new one-pot procedure for the efficient synthesis of novel 3,4-dihydrocoumarin derivatives using commercially available substituted 2-hydroxybenzaldehydes, Meldrum's acid, and isocyanides by a three-component condensation reaction in dichloromethane at room temperature without using any catalysts and activation was developed.     

Facile sonochemical synthesis of tellurium and tellurium dioxide nanoparticles: Reducing Te(IV) to Te via ultrasonic irradiation in methanol

In this study, tellurium (Te) nanostructures were synthesized via a facile sonochemical method by reducing TeCl₄ to Te under ultrasonic irradiation in methanol. Moreover, by carrying out the reaction in an alkaline environment TeO₂ nanoparticles were produced. According to our knowledge, it is the first time that without secondary reducing agent Te⁴⁺ are reduced to Te. Also, the effects of ultrasonic power, irradiation time, solvent, and surfactant on the morphology and particle size of Te nanostructures were investigated. The obtained products were characterized by XRD, SEM, EDS, FT-IR and DRS.     

Ultrasound-promoted synthesis of 1-amidoalkyl-2-naphthols via a three-component condensation of 2-naphthol, ureas/amides, and aldehydes, catalyzed by sulfamic acid under ambient conditions

A three-component one-pot condensation of 2-naphthol, ureas/amides and aldehydes catalyzed by sulfamic acid, under ultrasound irradiation and ambient conditions gives 1-amidoalkyl-2-naphthols in excellent yield and in short time.     

A three-component cyclocondensation reaction for the synthesis of new triazolo[1,5-a]pyrimidine scaffolds using 3-aminotriazole,aldehydes and ketene N,S-acetal

Molecular Diversity - This study describes the use of 3-aminotriazole, different aldehydes and N-methyl-1-(methylthio)-2-nitroethenamine as a ketene N,S-acetal in a three-component condensation for...     

Particle imaging techniques for volumetric three-component (3D3C) velocity measurements in microfluidics

Abstract  

The reliable measurement of the 3D3C velocity field in microfluidic devices becomes more and more important for future optimization and developments for lab-on-a-chip applications or point-of-care medical diagnosis systems. In the past years, different particle-based imaging methods, such as confocal scanning microscopy, holography, stereoscopic and tomographic imaging or approaches based on defocused particle images or optical aberrations have been developed and applied successfully to measure velocity fields in microfluidic systems. The benefits and drawbacks of these methods will be discussed in detail as the proper understanding of the measurement principle is essential to select the most appropriate technique for a desired measurement application. Once an imaging method is chosen, the velocity can be estimated by correlation-based methods or tracking approaches. The advantages and disadvantages of both methods and the importance of image preprocessing will also be discussed in detail.     

One-pot three-component synthesis of 3-hydroxy-5,5-dimethyl-2-[phenyl(phenylthio)methyl]cyclohex-2-enone derivatives under ultrasound

3-Hydroxy-5,5-dimethyl-2-[phenyl(phenylthio)methyl]cyclohex-2-enone is synthesized via one-pot three-component reactions of aromatic aldehyde, substituted thiophenol and 5,5-dimethyl-1,3-cyclohexanedione catalyzed by p-dodecylbenzene sulfonic acid (DBSA) under ultrasound. Under ultrasound irradiation the yields are much higher (sometimes substantially, by almost double) and the reaction time decreases substantially, the reaction conditions are milder. This method provides several advantages such as environment friendliness, high yields and simple work-up procedure and the protocol provides a novel alternative for the synthesis of thioether.     

机械合金化合成CoSb3过程中的固相反应机理的热力学解释

用Co和Sb作为初始原料，通过机械合金化(mechanical alloying, MA)的方法合成了CoSb₃,并系统研究了MA转速和MA时间对MA过程中固相反应的影响.XRD结果表明，相同MA转速下，CoSb₃的量随MA时间的延长而增多，但是MA时间过长会导致大量CoSb₂的生成，甚至诱发CoSb₃分解为CoSb₂和非晶态Sb.而提高MA转速，只能缩短固相反应的发生时间，而不会改变整个固相反应 关键词： 机械合金化 热电材料 3')" href="#">CoSb₃ 非平衡热力学     

Ultrasound-assisted three-component synthesis of 3-(5-amino-1H-pyrazol-4-yl)-3-(2-hydroxy-4,4-dimethyl-6-oxocyclohex-1-enyl)indolin-2-ones in water

Indium(III) chloride was found to be an efficient catalyst for the synthesis of 3-(5-amino-1H-pyrazol-4-yl)-3-(2-hydroxy-4,4-dimethyl-6-oxocyclohex-1-enyl)indolin-2-ones by one-pot, three-component reaction of dimedone, 1H-pyrazol-5-amines and isatins in water under ultrasonic irradiation. The advantages of this method are the use of a readily available catalyst, easy workup, excellent yields, and the use of water as a solvent that is considered to be relatively environmentally benign.     

Facile synthesis and characterization of Co nanoplatelets with tunable dimensions via solution reduction process

Plate-like Co nanoparticles with different sizes were synthesized by solution reduction process. The size of Co nanoplatelets can be tuned by varying the concentration of CoCl₂·6H₂O and the dosage of N₂H₄·2H₂O. The Co nanoplatelets with the different size all exist in both fcc and hcp crystal structures. The normal direction of the nanoplatelets is perpendicular to the (002) planes of hcp phase or to the (111) planes of fcc phase. The saturation magnetizations of the samples are lower than the corresponding bulk value. The coercivities of the samples vary with the phase content and the particle size. The shape control mechanism was discussed.