稀土发光材料的合成方法

简要介绍了合成稀土发光材料的6种方法,包括水热合成法、溶胶-凝胶法、微波辐射法、燃烧合成法以及共沉淀法。参考文献31篇。     

无机纳米材料的光化学合成

无机纳米材料的合成是纳米科学发展的前提和基础之一。区别于传统的高温湿化学合成法,光化学方法在无机纳米材料的合成中表现出许多优点,并在近年来受到了广泛关注。本文分三个部分综述了近年来光化学方法在无机纳米材料合成中的应用,具体包括贵金属纳米材料的光化学合成与负载,半导体纳米材料的光化学合成以及表面等离子体共振诱导的各向异性金属纳米晶合成。最后,在总结光化学方法在无机纳米材料合成中体现出的优势及目前研究仍存在不足的基础上,我们对其未来可能的发展方向进行了展望。     

离子热法合成分子筛的研究进展

离子热法是以离子液体或低共熔混合物为介质的一种新型的分子筛合成方法, 它提供了一种离子态的独特合成环境, 为合成新型分子筛及研究分子筛的生成机理提供了机会. 本文综述了离子热法在分子筛合成方面取得的一些进展, 包括合成方法的创新、合成机理的研究、新材料的合成以及新型催化剂的制备等, 并展望了其发展前景.     

Solid-phase synthesis of polyfunctional polylysine dendrons using aldehyde linkers

A straightforward method for the solid-phase synthesis of C-terminally modified polylysine dendrons has been developed by applying bisalkoxybenzaldehyde and trisalkoxybenzaldehyde linkers. The method has been used for the synthesis of polylysine dendrons with a variety of C-terminal ‘tail groups’ such as alkyl, propargyl, and dansyl to give dendrons in high crude purity. Furthermore, the method was successful for the synthesis of dendrons with multiple N-terminal pentapeptide groups together with C-terminal alkyl and propargyl tail groups. Finally, the method was shown to be well-suited for automated synthesis.     

微波固相法合成钠快离子导体Na5YSi4O12

应用微波方法合固相反应难于制备的Ｎａ５ＹＳｉ４Ｏ１２纯相，讨论了微波合成条件对产物的影响，与溶胶－凝胶法相比，微波法反应速率快，选择性强，合成的样品具有特异的聚集态，缺陷和微结构，从而导致离子导电活化能下降。     

Synthesis of Zn/Al mixed-oxide catalyst for carbonylation of glycerol with urea

Zn/Al mixed oxide was prepared by the coprecipitation or the hydrothermal method under different conditions and used as catalyst for synthesis of glycerol carbonate by carbonylation of glycerol with urea. The physical properties of the prepared Zn/Al mixed oxide particles were investigated, as well as their activity as catalyst in the mentioned synthesis. The dried Zn/Al mixed-oxide particles prepared by the coprecipitation method showed higher activity in synthesis of glycerol carbonate than those prepared by the hydrothermal method. The Zn/Al mixed oxide prepared by the coprecipitation method without NaNO₃ showed the highest catalytic activity in synthesis of glycerol carbonate.     

A new RNA synthetic method with a 2'-O-(2-cyanoethoxymethyl) protecting group

A novel method for the synthesis of RNA oligomers with 2-cyanoethoxymethyl (CEM) as the 2'-hydroxyl protecting group has been developed. The new method allows the synthesis of oligoribonucleotides with an efficiency and final purity comparable to that obtained in DNA synthesis. [structure: see text]     

Cascade Multicomponent Synthesis of Indoles,Pyrazoles, and Pyridazinones by Functionalization of Alkenes

The development of multicomponent reactions for indole synthesis is demanding and has hardly been explored. The present study describes the development of a novel multicomponent, cascade approach for indole synthesis. Various substituted indole derivatives were obtained from simple reagents, such as unfunctionalized alkenes, diazonium salts, and sodium triflinate, by using an established straightforward and regioselective method. The method is based on the radical trifluoromethylation of alkenes as an entry into Fischer indole synthesis. Besides indole synthesis, the application of the multicomponent cascade reaction to the synthesis of pyrazoles and pyridazinones is described.     

Chemical Synthesis of Native S-Palmitoylated Membrane Proteins through Removable-Backbone-Modification-Assisted Ser/Thr Ligation

The preparation of native S-palmitoylated (S-palm) membrane proteins is one of the unsolved challenges in chemical protein synthesis. Herein, we report the first chemical synthesis of S-palm membrane proteins by removable-backbone-modification-assisted Ser/Thr ligation (RBM^GABA-assisted STL). This method involves two critical steps: 1) synthesis of S-palm peptides by a new γ-aminobutyric acid based RBM (RBM^GABA) strategy, and 2) ligation of the S-palm RBM-modified peptides to give the desired S-palm product by the STL method. The utility of the RBM^GABA-assisted STL method was demonstrated by the synthesis of rabbit S-palm sarcolipin (SLN) and S-palm matrix-2 (M2) ion channel. The synthesis of S-palm membrane proteins highlights the importance of developing non-NCL methods for chemical protein synthesis.     

小分子抗原人工合成进展

小分子免疫分析技术的应用日渐广泛,合成稳定的、具有良好免疫原性的人工抗原是制备单克隆抗体和建立免疫分析方法的前提和关键。 本文对国内外半抗原的设计与合成方法、载体的选择、半抗原与载体的耦联方法等进行了综述,并对小分子抗原人工合成中相关的问题进行了讨论。     

Tandem SN2-Michael addition to vinylogous carbonates for the stereoselective construction of 2,3,3,5-tetrasubstituted tetrahydrofurans

A stereoselective method for the synthesis of substituted tetrahydrofuran derivatives employing a tandem alkylation-Michael addition sequence to vinylogous carbonates is developed. The method could be used to synthesize THFs bearing tertiary ethers. Further, the method is extended to the synthesis of adjacent bis-THFs.     

Novel diphenylmethyl-Derived Amide Protecting Group for Efficient Liquid-Phase Peptide Synthesis: AJIPHASE

An efficient method for the synthesis of peptides bearing an amide at the C-terminal is described. This method involves the attachment of a C-terminal protecting group bearing long aliphatic chains, followed by the repetition of simple reaction and precipitation steps with the combined advantages of liquid-phase peptide synthesis (LPPS) and solid-phase peptide synthesis (SPPS). Using this method, a hydrophobic peptide was successfully synthesized in good yield and high purity, which cannot be obtained satisfactorily by SPPS.     

The Microwave‐Assisted Ionic‐Liquid Method: A Promising Methodology in Nanomaterials

In recent years, the microwave‐assisted ionic‐liquid method has been accepted as a promising methodology for the preparation of nanomaterials and cellulose‐based nanocomposites. Applications of this method in the preparation of cellulose‐based nanocomposites comply with the major principles of green chemistry, that is, they use an environmentally friendly method in environmentally preferable solvents to make use of renewable materials. This minireview focuses on the recent development of the synthesis of nanomaterials and cellulose‐based nanocomposites by means of the microwave‐assisted ionic‐liquid method. We first discuss the preparation of nanomaterials including noble metals, metal oxides, complex metal oxides, metal sulfides, and other nanomaterials by means of this method. Then we provide an overview of the synthesis of cellulose‐based nanocomposites by using this method. The emphasis is on the synthesis, microstructure, and properties of nanostructured materials obtained through this methodology. Our recent research on nanomaterials and cellulose‐based nanocomposites by this rapid method is summarized. In addition, the formation mechanisms involved in the microwave‐assisted ionic‐liquid synthesis of nanostructured materials are discussed briefly. Finally, the future perspectives of this methodology in the synthesis of nanostructured materials are proposed.     

Palladium-Catalyzed Allylic C-OH Functionalization for Efficient Synthesis of Functionalized Allylsilanes

A new method is described for palladium-catalyzed allylic silylation using allylic alcohols and disilanes as precursors. The reactions proceed smoothly under mild and neutral conditions, and this method is suitable for synthesis of regio- and stereodefined allylsilanes. The presented silylation reaction can be easily extended to include synthesis of allylboronates by change of the dimetallic reagent. The presented synthetic procedure offers a broad platform for the selective synthesis of functionalized allyl metal reagents, which are useful precursors in advanced organic chemistry and natural product synthesis.     

The Ampoule Method: A Pathway towards Controllable Synthesis of Electrocatalysts for Water Electrolysis

The ampoule method provides a promising pathway towards the controllable synthesis of novel electrocatalysts for water electrolysis due to its straightforward manipulation of reaction conditions, accessible experimental design, and controlled environment. This Concept introduces the development of the ampoule method and anticipates its application in electrocatalyst synthesis for water electrolysis. First, the history, device configuration, and merits of the ampoule method are briefly introduced. Afterwards, typical materials synthesized by the ampoule method are discussed. Then, recent process in applying the ampoule method to synthesize electrocatalysts for water electrolysis is highlighted. Finally, opportunities and potentials of this method in facilitating electrocatalyst synthesis for water electrolysis are discussed.     

季铵碱的合成研究进展

简要综述了季铵碱的5种合成方法,包括氧化银法、碱置换法、离子交换树脂法、双极膜电渗析法和电解法（电膜反应器法）。对比分析了各种合成方法的优势与局限性,并对其未来的发展前景进行了展望。     

Combinatorial liquid-phase synthesis of

A new method for the synthesis of [1,4]oxazepin-7-ones from readily available aldehydes and alpha-amino alcohols was developed using the Baylis-Hillman reaction as the key step. To determine the scope and limitations of the method, a mixture library was synthesized from six aldehydes and six alpha-amino alcohols on the soluble polymer support poly(ethylene glycol) 5000 monomethyl ether (MeOPEG) via split synthesis and analyzed by GC-EIMS. Those oxazepines that were formed predominantly were resynthesized in a parallel synthesis and fully characterized. Thus, we have shown that split synthesis on MeOPEG can be an efficient method to rapidly screen the substrate spectrum of a newly developed reaction sequence.     

A facile synthesis of cyclic bis(3′→5′)diguanylic acid

This paper describes a new method for synthesizing biologically important cyclic bis(3′→5′)diguanylic acid (cGpGp) in a higher yield than that of the existing synthetic method. In the new synthesis, the following two means, in place of those used in the existing synthesis are employed as main strategies to cause the increase in product yield. One of these distinctive strategies in the new synthesis is that the phosphoramidite method is used for the preparation of a key synthetic intermediate of a linear guanylyl(3′→5′)guanylic acid derivative. This method allowed higher-yield formation of the intermediate than that by the triester method used in the existing synthesis. The second distinctive strategy used in the new synthesis is that allyloxycarbonyl and allyl groups are used for the protection of two guanine bases and two internucleotide bonds, respectively. These four allylic protectors can be removed all at once by the organopalladium-catalyzed reaction under neutral conditions. Thus, deprotection of the protected cGpGp precursor was achieved in the present synthesis in a shorter step and under milder conditions than the deprotection achieved in the existing synthesis, which uses diphenylacetyl and o-chlorophenyl groups as protectors for two guanine bases and two internucleotide bonds, respectively, whose full removal requires two different procedures including rather harsh basic treatment. As a result, technical loss and decomposition of the target product in the new synthesis is remarkably reduced.     

Direct, facile synthesis of acyl azides and nitriles from carboxylic acids using bis(2-methoxyethyl)aminosulfur trifluoride

A mild, efficient, and practical method for the one-step synthesis of acyl azides from carboxylic acids using bis(2-methoxyethyl)aminosulfur trifluoride is described. The reaction was easily extended to the synthesis of the corresponding nitriles by the inclusion of phosphorous reagents. The method can be applied to the synthesis of optically active nitriles in high yields, and is compatible with fluorous phosphines.