Simple Protocol for Synthesis and Cleavage of Tetrahydropyranyl Ethers Using FeSO4 as an Inexpensive Catalyst

Protection and deprotection of alcohols and phenols as tetrahydropyranyl ethers (THP ethers) using an hydrous FeSO₄ under microwave irradiation without solvent is carried out.     

十二烷基硫酸钠为模板制备ZnO纳米管新方法的研究

自从1991年日本科学家Iijim a发现碳纳米管以来,在纳米管制备和理论方面的研究引起了广泛的关注[1]。管状、线状、棒状、带状、针状等一维纳米结构已成为世界各国研究人员关注的焦点[2￣6]。究其原因在于其特殊的物理性质,对于纳米领域的基础研究有新的启发作用,这些一维纳米结     

Synthesis of Novel Unsaturated Alkyl Ethers of Racemic Deoxyisopodophyllotoxin as Cytotoxic Agents

Recently, some lignans in different subgroups have been found to possess an isopentenyl-derived side chain with certain bioactivities1-3. For example, 7-O-(3- methyl-2-bytenyl)-isodaurinol 1, isolated from Haplophyllum myrtifolium by G?zler and co-workers…     

Kinetics and mechanism of processes in the system FeSO4·7H2O-MnO2

Processes which occur during the thermal treatment of system FeSO₄·7H₂O-MnO₂ are of the interest for obtaining MnSO₄, which can be easily soluted in water and separated from impurities in manganese slime in zinc metallurgy. Results of the experimental investigations of such processes are given in this paper. Kinetic parameters for the previously defined mechanism were determined using Borchardt and Daniels method.     

TG/DTA/MS Study of the thermal decomposition of FeSO4·6H2O

The thermal decomposition of FeSO₄·6H₂O was studied by mass spectroscopy coupled with DTA/TG thermal analysis under inert atmosphere. On the ground of TG measurements, the mechanism of decomposition of FeSO₄·6H₂O is: i) three dehydration steps FeSO₄·6H₂O FeSO₄·4H₂O+2H₂O FeSO₄·4H₂O FeSO₄·H₂O+3H₂O FeSO₄·H₂O FeSO4+H₂O ii) two decomposition steps 6FeSO₄ Fe₂(SO₄)₃+2Fe₂O₃+2SO₂ Fe₂(SO₄)3 Fe₂O₃+3SO₂+3/2O₂ The intermediate compound was identified as Fe₂(SO₄)₃ and the final product as the hematite Fe₂O₃.     

Isothermal investigation of decomposition of FeSO4·H2O-BaO2 mixtures

Isothermal studies were conducted on mixtures of Fe₂SO₄·H₂O in BaO₂ in molar ratios ofn=4, 2 and 1 at temperatures of 573 and 1073 K, in a closed crucible, in air as gas medium. The solid products of decomposition were investigated by means of X-ray analysis, Mössbauer spectroscopy and electron spectroscopy.The experiments revealed that the mechanism of the process is connected with the formation of different quantities of barium ferrites (BaFeO₃, BaFe₂O₄ and BaFe₁₂O₁₉), as well as BaSO₄ and Fe₂O₃, depending on the quantity of BaO₂ in the initial mixture, the partial pressure of the gas components and temperature. Differences were found in the mechanism of the process for the same mixtures under dynamic temperature conditions.     

Novel and Efficient Oxidation of Benzyl Ethers to Benzaldehydes by DMSO/49% Aq. HBr

Dimethylsulfoxide (DMSO) oxidizes benzyl ethers into corresponding benzaldehydes at 110°C; the reaction is accelerated by 49% aq. HBr. The conditions work well for different aryl‐substituted benzyl ethers. This protocol is inert toward dialkyl ethers.     

Raman spectroscopic investigation of aqueous FeSO4 in neutral and acidic solutions from 25‡C to 303‡C: inner- and outer-sphere complexes

Raman spectra of aqueous FeSO₄ and (NH₄)₂SO₄ solutions have been recorded over broad concentration and temperature ranges. Whereas the v₁-SO ₄ ^2- band profile is symmetrical in noncomplexing (NH₄)₂SO₄ solutions, in FeSO₄ solutions a shoulder appears on the high-frequency side, which increases in intensity with increasing concentration and temperature. The molar scattering coefficient of the v_1-SO ₄ ^2- band is the same for all forms of sulfate in (NH₄)₂SO₄ and FeSO₄ solutions and is independent of temperature up to 150‡C, the highest temperature studied. The high-frequency shoulder is attributed to the formation of a contact ion pair, Fe²⁺OSO^3/2-, as is the splitting of the v_3-SO ₄ ^2- antisymmetric stretching mode which is observed in the FeSO₄ solution. The bending modes v_2-SO ₄ ^2- and v_4-SO ₄ ^2- , normally forbidden in the isotropic spectrum, show a gain in intensity with increasing ion-pair formation. A polarized band has been assigned to the Fe²⁺-O ligand vibration. No higher associates or anionic complexes are required to interpret the spectroscopic data. No evidence of contact ion pairing between Fe²⁺ and HSO4 ₄ ^- could be detected at temperatures up to 303‡C in 1 molal solutions of FeSO₄ with an excess of 2 molal H₂SO₄.     

Highly Efficient System for Reduction of Carboxylic Acids and Their Derivatives to Alcohols by HfCl4/KBH4

HfCl₄/KBH₄ was found to be a facile, efficient, convenient, and chemoselective system for the reduction of carboxylic acids and their derivatives to the corresponding alcohols under mild conditions. HfCl₄/NaBH₄ was also utilized to reduce the same carboxylic acids and their derivatives, and it was found that the reducing ability of HfCl₄/NaBH₄ was similar to that of HfCl₄/KBH₄. The action of HfCl₄/KBH₄ on other types of substrates, such as benzyl chloride, peracid, epoxide, ketone, amide, imine, pyridine-N-oxide, and nitrile, was investigated, too. In addition, some competitive reductions of styrene oxide in the presence of carboxylic acid, carboxylic ester, nitrile, and amide were achieved.     

Transformation of Primary Benzyl Amines to Benzyl Esters

Primary benzyl amines, upon treatment with aq. NaNO₂ and appropriate organic acids at 0–5°C, give their respective benzyl esters.     

A New Method for the Preparation of Co3O4 Nanoparticles

In this study, a novel method was used to prepare well-separated and spherical tricobalt tetraoxide (Co₃O₄) nanosized particles. The overall process involves three steps: preparation of insoluble carboxyl-containing grafted starch copolymer (ISC), formation of precursor (ISC-Co), decomposition of ISC-Co, and phase transition of Co₃O₄ nanoparticles. The Infrared spectra used for ISC and ISC-Co are discussed. The decomposition of the precursor was studied by thermogravimetric-differential thermal analysis, the crystalline phase was characterized by x-ray diffraction, and the size distribution and shape of particles were observed by transmission electron microscopy. Translated from Journal of Northwest Normal University (Natural Science Edition), 2005, 5(5) (in Chinese)     

分子内桥连有机钴配合物的合成及热稳定性研究

The intramolecularly bridged alkyl cobaltic complexes are one of important coenzyme B₁₂ model coplexes. In this paper, study on the thermolytic reaction of aqua(3-bromopropyl)cobaloximes in solution revealed that a new intramolecularly bridged alkyl cobaloximes complex was formed and the reaction is influenced by tempertature and solvent. Adding cyclodxtrin has no obvious effect to the rate of the reaction, but various products with different axial bases were obtained. The intramolecularly bridged alkyl cobaloxime complex (bromo(O-trimethylene-dimethy- lglyoxime)(dimethylglyoximate)cobalt(Ⅲ)) was characterized by EA and ESI-MS. Thermogravimetric analysis of this complex found that a carbon radical that from homolysis of the Co-C bond is retained in the proximity of Co^Ⅱ- complex, which is very similar to the behavior of coenzyme B₁₂.     

Silica Sulfuric Acid as an Efficient Reagent for the Synthesis of Symmetrical Ethers Under Mild and Heterogeneous Conditions

A mild and efficient method for the synthesis of symmetrical ethers using silica sulfuric acid is reported. All reactions are performed under compeletly heterogeneous conditions in good to high yields.     

Ag-Pd/g-C3N4的制备及在水溶液中选择性氧化苯甲醇

采用硼氢化钠还原法在g-C₃N₄的表面负载Ag和Pd纳米颗粒制备Ag/g-C₃N₄、Pd/g-C₃N₄、Ag-Pd/g-C₃N₄光催化剂.采用能谱仪、X射线衍射、高分辨透射电子显微镜等技术对样品进行表征.结果显示,Ag-Pd/g-C₃N₄复合材料中C、N、Ag和Pd元素的质量百分数分别为22.718%、59.966%、9.132%和8.184%.Ag和Pd纳米颗粒负载在g-C₃N₄表面可提高材料在可见光区域的吸收以及提高苯甲醇的转化率,生成苯甲醛的选择性为85.6%.     

Simple and Efficient Method for the Protection of Hydroxyl Groups as 4-Methoxybenzyl Ethers

PMB ethers of alcohols are obtained in good yields and under mild conditions using the 4-methoxybenzyl N-allyl thiocarbamate and N-bromosuccinimide (NBS)/TfOH as the catalyst. The present method is very fast, simple, and efficient.     

The First Synthesis of Functionalized Oxacalix[4]crown Ethers

O-alkylation and cyclization of 25,27-dihydroxy-4,6,16,18-tetranitro-oxacalix[4]arene were performed with mono- and bifunctional alkylating agents under basic conditions. In this way several 1,3-alt oxacalix[4]crown-4, 5 and 6 ethers were synthesized and characterized     

Synthesis of Benzyl Alkyl Ethers by Intermolecular Dehydration of Benzyl Alcohol with Aliphatic Alcohols under the Effect of Copper Containing Catalysts

Synthesis of benzyl alkyl ethers was performed in high yields by intermolecular dehydration of benzyl and primary, secondary, tertiary alcohols under the effect of copper containing catalysts. The formation of benzyl alkyl ethers occurs with participation of benzyl cation.     

Synthesis of Diaryl Ethers Through the Copper-Catalyzed Arylation of Phenols with Aryl Iodides Using KF/Al2O3

An efficient synthesis of diaryl ethers by the copper-catalyzed arylation of phenols with a variety of aryl iodide susing KF/Al₂O₃ as a suitable base and CuI and 1,3 diphenyl-1,3 propandione as the catalyst is described.     

Sr2CeO4∶Eu3+柠檬酸-凝胶法的合成及发光性质研究

柠檬酸-凝胶方法促使多离子在分子水平上混合，与固相烧结方法相比，能够降低烧结温度和烧结时间。利用这种方法在1000℃下很短的时间得到单相化合物Sr₂CeO₄。Sr₂CeO₄是一种发出很强蓝光的基质发光材料。为寻找新的发光体，我们将稀土离子Eu³⁺掺杂在其中，从荧光光谱上可以看出存在从基质向稀土离子的能量转移。Sr₂CeO₄∶Eu³⁺的发光颜色可调谐，当Eu³⁺离子浓度较小(< 0.5mol%)时，体系发出很强的白光;当Eu³⁺离子浓度较大(>10mol%)时，体系发出很强的红光，并且猝灭浓度高。