Gold(I)-catalysed iodoalkoxylation of allenes

Gold(I)-catalysed intermolecular iodoalkoxylation of allenes occurs in a regioselective and stereoselective manner to produce versatile iodo-tert-allyllic ether products. The products can be further elaborated through cross-couplings to yield highly substituted tert-allylic ethers.     

Desymmetric hydrogenation of a meso-cyclic acid anhydride toward biotin synthesis

Catalytic reactivity in the hydrogenation of a cyclic anhydride to a biotin synthetic intermediate has been investigated on the basis of Lyons’ original method using Wilkinson Ru complex, revealing the high performance of DPPF and XANTPHOS diphosphines possessing wide bite angles. The results have shown a new trail for design of the corresponding asymmetric catalysts, and the potential utility of (S,S)-Et-FerroTANE and (S,S)-(R,R)-Ph-TRAP has been demonstrated.     

1,n-Diamines. Part 3: Microwave-assisted synthesis of N-acyl-N′-arylhexahydropyrimidines and hexahydro-1,3-diazepines

In this Letter we present a method for the synthesis of N-acyl-N′-arylhexahydropyrimidines 1, by ring closure of N-acyl-N′-aryl-1,3-propanediamines 3 with formaldehyde. Cyclodehydrations were performed in aqueous medium under microwave irradiation, and led to high yields of the desired compounds in remarkably short reaction times. The method also allowed for the synthesis of hitherto unreported N-acyl-N′-arylhexahydro-1,3-diazepines 2. The acyclic tetramethylenic precursors 4 were synthesized by selective functionalization of N-arylputrescines.     

Direct palladium/carboxylic acid-catalyzed C-allylation of cyclic 1,3-diones with allylic alcohols in water

The direct activation of C-O bonds in allylic alcohols in water as a suspension medium by palladium complexes has been accelerated by carrying out the reactions in the presence of a carboxylic acid. The palladium-catalyzed allylation of cyclic 1,3-diones using allylic alcohols directly gave the corresponding C-allylated products in good yields.     

Synthetic,spectroscopic, fluorescence,and biological investigation of Co(II), Ni(II), Cu(II), and Zn(II) complexes of Schiff bases derived from 3-formyl-2-mercaptoquinolines (Quinol-2-thiones)

Co(II), Ni(II), Cu(II), and Zn(II) complexes have been prepared with Schiff bases derived from 3-formyl-2-mercaptoquinoline and substituted anilines. The prepared Schiff bases and chelates have been characterized by elemental analysis, molar conductance, magnetic susceptibilities, electronic, IR, ¹H-NMR, ESR, cyclic voltammetry, FAB-mass, and thermal studies. The complexes have stoichiometry of the type ML₂ · 2H₂O coordinating through azomethine nitrogen and thiolate sulfur of 2-mercapto quinoline. An enhancement in fluorescence has been noticed in the Zn(II) complexes whereas quenching occurred in the other complexes. The ligands and their metal complexes have been screened in vitro for antibacterial and antifungal activities by MIC methods with biological activity increasing on complexation. Cu(II) complexes show greater bacterial than fungicidal activities. The brine shrimp bioassay was also carried out to study the in vitro cytotoxicity properties of the ligands and their corresponding complexes. Only four compounds have exhibited potent cytotoxic activity against Artemia salina; the other compounds were almost inactive for this assay.     

Electrochemical behavior of PbO2/PbSO4 electrode in the presence of surfactants in electrolyte

The electrochemical behavior of PbO₂/PbSO₄ electrode is investigated in 4.5 M H₂SO₄ in presence of three surfactants, Sodium Dodecyl Sulfate (SDS), Cetyltrimethylammonium bromide (CTAB) and Sodium tripolyphosphate (STPP), using cyclic voltametry, electrochemical spectroscopy impedance and galvanostatic discharge as techniques. The micro morphology of the surface of the modified PbO₂ electrodes is examined by scanning electron microscopy. The results show that SDS and CTAB when added in the electrolyte could refine the coating particles and change the roughness of the surface of the electrode leading to a thin film of PbO₂ with amorphous character. In addition, SDS and CTAB shift the hydrogen evolution potential towards more negative values, improve the discharge capacity of the anodic layer and accelerate the charge transfer. Under cathodic polarization, CTAB presents the lowest value of the charge transfer resistance R_ct. In the contrary, STPP shifts the oxygen evolution potential towards more positive values, passivates the surface of the electrode and inhibits completely the reaction of PbO₂ formation.     

反射式薄层可见光谱电解池的制作与性能测试

设计制作了一种反射式薄层可见光谱电解池。该电解池采用光亮铂片作为工作电极,将铂丝辅助电极和Ag AgCl参比电极组装在一起。薄层池中间的溶液薄层是通过光亮铂片和覆盖其上的玻璃片之间的塑料薄膜垫圈加以控制,当液层厚度为0.2mm时,液层容积为16μL。由于采用双平行反射的光路,使入射光与出射光保持在一直线上,可以在不变更光路系统下的各种光度计上使用。在K3Fe(CN)6 K4Fe(CN)6体系中,用循环伏安法、恒电位现场光度法进行性能测试。实验结果表明,该电池具有良好的薄层光谱电化学性能,可用于薄层可见光谱电化学研究。     

Synthesis,characterizations, and electrochemical studies of ZnO/reduced graphene oxide nanohybrids for supercapacitor application

Herein the present article reports the fabrication of ZnO/reduced graphene oxide (ZnG) nanohybrid following a reduction-based process using a non-hazardous material, i.e., ascorbic acid. The morphology, structure, and bonding in the nanohybrid were analyzed using different techniques. Atomic force microscopy and scanning electron microscopy images show spherical particles of ZnO distributed over reduced graphene oxide (rGO). The X-ray diffraction analysis gives calculated values of crystallite size for ZnO as 15.62 nm. The successful incorporation of ZnO nanoparticles into rGO was confirmed using energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy analyses. The electrochemical studies were performed using an electrolyte (0.5 M H₂SO₄). The calculated value of specific capacitance for the nanohybrid was 345 Fg^-1, which was found to be almost double as compared to that of rGO, which is having a value of only 190.5 Fg^-1 at the same scan rate. The nanohybrid also showed excellent capacitance retention after 1,000 cycles.     

环状膦酸酯的合成及其质谱特征

本文研究了环状膦酸酯的合成方法，通过三种方法合成了十五个具有各种烷基结构的六元和七元环膦酸酯，并对这十五个化合物质谱作了分析和归纳，得出了一些有助于鉴定这类膦酸酯的质谱特征。