APPLICATION OF THE SULFONATE ESTER GROUP AS A LINKER FOR SOLID PHASE ORGANIC SYNTHESIS

A use of Sulfonate ester as a linker in synthesis of (-aminoalkanols was reported. Diols were tethered onto polystyryl sulfonyl chloride resin, yielding sulfonate resins (2). After cleaved by diethyl amine, diisopropylamine and propylamine respectively, three (-aminoalkanols were obtained.

Solid-phase Synthesis of-Haloaldehydes from Polymer-supported 4-(Phenylseleno)morpholine

Polystyrene-supported 4-(phenylseleno)morpholine was synthesized and could be used as an efficient ?selenenylating agent for saturated aldehydes. ?Haloaldehydes were prepared by reaction of polystyrene-supported ?selenoaldehydes with bromine or sulfuryl chloride in good yield and high purity.

Solid-Phase Stereoselective Synthesis of (E)-1, 2-Disubstituted Ethenes from Polymer-Sopported a-Selenoaldehydes

Reaction of polymer-supported a-selenoaldehydes with Grignard reagents afforded polymer-bound B-hydroxyalkyl selenides, which treated with thionyl chloride and triethylamine leading to (E)-1, 2-disubstituted ethenes in good yield.

Traceless solid-phase synthesis of 3-substituted isoxazoles from polystyrene-supported vinyl selenide

A novel facile procedure for traceless solid-phase synthesis of 3-substituted isoxazoles in good yields and with excellent purities using polymer-supported vinyl selenide has been developed.

Solid-Phase Synthesis of Acrylamide Using Polymer-Supported β-Selenopropionic Acid

A novel polystyrene-supported ?selenopropionic acid has been developed and applied to facile synthesis of acrylamides.

Solid-phase synthesis of (Z)-allyl iodides from 3-acetoxy-2-methylene-alkanoates with recyclable polymer-supported selenium bromide

Reaction of polystyrene-supported lithium selenide with 3-acetoxy-2-methylene-alkanoates afforded the corresponding allyl selenide resins and subsequent cleavage from the polymer by treating with methyl iodide to furnish （Z）-allyl iodides in good yields and high purities. The polymeric selenium reagent can be regenerated and reused. So it is a environmentally benign reagent.

Solid-phase Synthesis of Unsaturated β-Dicarbonyl Compounds from Polymer-supported 4-(Phenylseleno)morpholine

The solid-phase synthesis of unsaturated ?dicarbonyl compounds has been reported.

Liquid-phase synthesis of Li_(2)S and Li_(3)PS_(4) with lithium-based organic solutions

Sulfide solid electrolytes are widely regarded as one of the most promising technical routes to realize all-solid-state batteries(ASSBs)due to their high ionic conductivity and favorable deformability.However,the relatively high price of the crucial starting material,Li_(2)S,results in high costs of sulfide solid electrolytes,limiting their practical application in ASSBs.To solve this problem,we develop a new synthesis route of Li_(2)S via liquid-phase synthesis method,employing lithium and biphenyl in 1,2-dimethoxyethane(DME)ether solvent to form a lithium solution as the lithium precursor.Because of the comparatively strong reducibility of the lithium solution,its reaction with sulfur proceeds effectively even at room temperature.This new synthesis route of Li_(2)S starts with cheap precursors of lithium,sulfur,biphenyl and DME solvent,and the only remaining byproduct(DME solution of biphenyl)after the collection of Li_(2)S product can be recycled and reused.Besides,the reaction can proceed effectively at room temperature with mild condition,reducing energy cost to a great extent.The as-synthesized Li_(2)S owns uniform and extremely small particle size,proved to be feasible in synthesizing sulfide solid electrolytes(such as the solid-state synthesis of Li_(6)PS_(5)C_(l)).Spontaneously,this lithium solution can be directly employed in the synthesis of Li_(3)PS_(4) solid electrolytes via liquid-phase synthesis method,in which the centrifugation and heat treatment processes of Li_(2)S are not necessary,providing simplified production process.The as-synthesized Li_(3)PS_(4) exhibits typical Li+conductivity of 1.85×10^(-4) S·cm^(-1) at 30℃.

Solid-phase Synthesis of Vinyl Sulfones Using Polystyrene-supported Selenomethyl Phenyl Sulfone

The solid-phase preparation of vinyl sulfones via a novel polystyrene-supported selenomethyl phenyl sulfone reagent has been reported.

Solid-phase Synthesis of Diethyl Trans-1-Aklenephosphonates Using Polymer-bound α-Diethoxyphosphoryl Methyl Selenide

The solid-phase preparation of diethyl trans-1 -alkenephosphonates via seleno-polymer reagent has been reported.

An Efficient Synthesis of Cyclopeptides Bridged with Aliphatic-aryl Ether Bond

Based on the pseudo-dilution effect (PDE) on solid support, three cyclopeptides with an aliphatic-aryl ether bond as the bridge were synthesized via SN2 reaction between bromoacetylated at N-terminal and the phenol –OH group in C-terminal Tyr residue. All the products were obtained in good overall yields and characterized by related analytic data.

Solid-Phase Organic Synthesis of Aryl Vinyl Ethers Using Sulfone-Linking Strategy

A novel facile solid-phase organic synthesis of aryl vinyl ethers by reaction of polystyrene-supported 2-phenylsulfonylethanol with phenols under Mitsunobu conditions and subsequent elimination reaction with DBU has been developed. The advantages of this method include straightforward operation, good yield and high purity of the products. Alternatively, a typical example of Suzuki coupling reaction on-resin was further applied to prepare 4-phenylphenyl vinyl ether for extending this method.

Wittig反应实验的绿色化改进

传统的有机化学实验教学中,大多侧重实验技能的训练,设置实验内容时对实验安全性、经典性和可重复性等因素考虑较多,而对反应的绿色化、新方法和新技能等重视程度不够。为此,经典的有机反应也需要不断改进,本文将需要在大量有机溶剂中进行的传统Wittig反应改进为无溶剂的固相研磨反应,使得合成方法更加简单、绿色、安全和高效。设计合成了3个不同推拉型(D-π-A)二苯乙烯结构分子,优化了反应条件,测定了它们的光谱性质,并对其进行比较,讨论其构性关系,不仅引入绿色化学理念,而且对知识进行扩展,增加了实验的新颖性、探索性和趣味性,提升了学生创新能力。

固废资源合成堇青石工艺及其性能研究

为了合理利用固废资源、缓解资源紧张,根据堇青石的化学组成,以质量分数分别为12%的电熔镁砂收尘粉、40%的电熔刚玉收尘粉、48%的石英尾砂为原料,分别在1320、1350、1380、1390、1400、1410℃保温3 h煅烧,制备堇青石质耐火原料,研究了煅烧温度对堇青石试样相组成、显微结构、物理性能等的影响。结果表明:在1390℃之前,镁铝尖晶石和方石英逐渐反应生成堇青石直至方石英相完全消除,当煅烧温度达到1390℃时,试样中的堇青石相含量达94%(w),次晶相为镁铝尖晶石,此时试样的热膨胀系数最低,为3.2×10^(-6)℃^(-1),体积密度较低,为1.85 g·cm^(-3),热导率较低,为1.279 W·(m·K)^(-1),显微结构较致密,综合性能最优。

氧化镧掺杂锰酸锂材料的制备及其电化学性能

采用高温固相合成法制备氧化镧掺杂的锰酸锂材料,研究了氧化镧不同掺杂比例(与二氧化锰的质量比分别为0%、0.5%、1.0%和1.5%)对样品性能的影响。实验结果表明:当氧化镧掺杂量为1%时,所制的锰酸锂材料在1 C下比容量最大,达到120.42 mAh/g;首次充放电效率最高,达96.76%;100次循环的1 C容量保持率最大,为90.28%。

固相法制备纳米CoMoO_(4)及其电化学性质研究

钼基金属氧化物因其较高的稳定性和质量比容量被视为一种极具潜力的超级电容器电极材料。本文采用固相化学合成法制备了纳米级CoMoO_(4)材料。结果表明,CMO-PEG2电极在1 A/g电流密度下具有较高的比电容,约为306.64 F/g,在10 A/g电流密度下循环10 000次后,初始可逆容量保持在75.75%,卓越的电化学性能归功于所合成的CoMoO_(4)所具有的一维纳米结构良好的导电性、相互支撑的纳米线结构以及理想的比表面积。本工作为CoMoO_(4)的合成及其在超级电容器中的应用提供了新的思路。

Mo掺杂La_(0.8)Sr_(0.2)Co_(1-x)Mo_(x)O_(3-δ)的电催化析氧、析氢性能研究

电解水制氢是一种清洁、高效和安全的技术,极具发展潜力的制氢手段。电解水制氢过程中,阳极析氧(OER)和阴极析氢(HER)动力学缓慢,需要较高的过电位突破能量壁垒,导致耗能较高。高效OER和HER催化剂的使用是提高电解水效率的关键,开发高活性、高稳定性和低成本的OER和HER双功能电催化剂,可极大促进电解水制氢的产业化发展。钙钛矿氧化物(结构式ABO_(3))电催化剂具有储量丰富、结构与成分易调控等优点,在电催化水分解制氢催化剂的研究中广受关注。钙钛矿氧化物的B位离子掺杂是增强其电催化活性的常见策略,合理选择B位掺杂元素的种类和含量,不仅可调控钙钛矿氧化物的晶体结构、获得更高的催化活性,还可赋予其双功能催化性能。以La_(0.8)Sr_(0.2)CoO_(3-δ)钙钛矿氧化物为原料,通过高价Mo离子掺杂,采用固相合成法制备了La_(0.8)Sr_(0.2)Co_(1-x)Mo_(x)O_(3-δ)(LSCM,x=0、0.05、0.1、0.2)系列钙钛矿材料,研究了Mo掺杂量(质量分数)对钙钛矿材料电催化析氧和析氢性能的影响。结果表明,掺杂少量Mo元素,不会改变LSCM的物相和微观形貌,但可有效提升OER和HER的催化活性,其主要原因是Mo掺杂改变了Co的价态、氧空位和晶体结构对称性。适量Mo元素掺杂对LSC钙钛矿氧化物的析氢和析氧性能均有提高,但随着Mo掺杂量增多,LSCM的OER和HER催化活性均开始下降。当Mo质量分数为5%时,La_(0.8)Sr_(0.2)Co_(0.95)Mo_(0.05)O_(3-δ)(LSCM-5)具有最优异的OER和HER催化活性,在10 mA·cm^(-2)电流密度下,OER和HER过电位分别为457和320 mV,Tafel斜率分别为89和32 mV·dec^(-1)。本研究证明,B位Mo掺杂,对开发低成本、高性能的析氢和析氧双功能钙钛矿氧化物电催化剂具有一定实用价值。

研磨法在固相有机合成中的应用

近几十年来有机工作者将研磨法用于固态有机合成,取得了一些成效,综述了近年来典型的固相有机研磨反应.

SAPO-34制备方法研究进展

综述了近年来SAPO-34分子筛制备方法的研究进展,介绍了超声处理、微波加热等技术在SAPO-34分子筛制备过程中的应用及原位合成、固相合成、气相合成和离子液体合成等新型制备方法。指出在不影响SAPO-34分子筛催化性能的前提下,降低合成低成本、减少环境污染、节水降耗是SAPO-34分子筛今后的开发方向。