Rapid,efficient and solvent-free synthesis of (un)symmetrical xanthenes catalyzed by recyclable sulfated polyborate

The present study describes a rapid, simple and straightforward approach to the synthesis of 1,8-dioxo-octahydroxanthenes, 14-phenyl-14H-dibenzo[a,j]xanthene and tetrahydrobenzoxanthene-11-ones under solvent-free conditions using sulfated polyborate as a highly efficient catalyst. The procedure offers several advantages including cleaner reaction profile, mild reaction condition, economic, recyclable and environmentally benign catalyst, high yields, simple experimental and workup procedures. While non-extractive work up/purification, along with reusability of catalyst make this method economically affordable for large scale.     

Crystal structure and pale‐yellow emitting properties of K3Gd1–xDyxB6O12 solid solutions

A new potassium dysprosium polyborate, K₃DyB₆O₁₂, has been prepared via the high‐temperature molten salt method and structurally characterized by single‐crystal X‐ray diffraction analysis. The structure can be described as a three‐dimensional framework composed of isolated bicyclic [B₅O₁₀]^5? groups and Dy³⁺ and K⁺ ions. The Fourier transform IR (FT–IR) and ultraviolet–visible (UV–Vis) spectra were investigated. A series of K₃Gd_1–xDy_xB₆O₁₂ phosphors was prepared and their photoluminescence properties were studied. The K₃Gd_1–xDy_xB₆O₁₂ phosphors exhibit a strong yellow emission band at 577 nm (the ⁴F_9/2→⁶H_13/2 transition of Dy³⁺) under UV excitation of 275 nm (the ⁸S_7/2→⁶I_J transition of Gd³⁺), suggesting the occurrence of the energy transfer Gd³⁺→Dy³⁺. The optimized doping concentration of the Dy³⁺ ion was 8 mol%. We may expect that K₃Gd_1–xDy_xB₆O₁₂ is a promising pale‐yellow emission phosphor for visual displays or solid‐state lighting.     

Expeditious and efficient synthesis of Strecker’s α-aminonitriles catalyzed by sulfated polyborate

A straightforward, mild, efficient, and environmentally benign protocol for a three-component Strecker reaction of aldehydes or ketones, amines, and trimethylsilyl cyanide catalyzed by sulfated polyborate has been described to afford α-aminonitriles under solvent-free reaction conditions. The major advantages of the present method are excellent yields, shorter reaction time, simple experimental procedure, easy workup procedure, recyclability of the catalyst, solvent-free reaction conditions and ability to tolerate a variety of functional groups which gives economical as well as ecological rewards.     

Oxidopolyborate chemistry: The self-assembled,templated, synthesis,and an XRD study of a 1-D coordination polymer, [Cu(en){B6O7(OH)6}].3H2O (en = 1,2-diaminoethane)

Abstract

[Cu(en){B₆O₇(OH)₆}]^.3H₂O (1) (en = 1,2-diaminoethane), obtained as a crystalline solid in low yield (31%) after prolonged standing of an aqueous solution initially containing [Cu(en)₂](OH)₂ and B(OH)₃ (1:7 ratio), was characterized by thermal analysis (TGA/DSC), ¹¹B NMR and IR spectroscopy, powder XRD, and single-crystal XRD studies, and magnetic susceptibility measurements. The single-crystal X-ray diffraction revealed that the oxidoborate complex is a 1D coordination polymer with the hexaborate(2-) ligand bridging two hexacoordinate Cu^(II) centers, in an alternating a fac-tridentate (κ³-O) and monodentate (κ¹-O) arrangement. Cu-O coordination bonds and extensive H-bonding networks promote and stabilize the self-assembly of [Cu(en){B₆O₇(OH)₆}]^.3H₂O from the Dynamic Combinatorial Libraries of available reactants. [Cu(en){B₆O₇(OH)₆}]^.3H₂O is thermally decomposed to CuB₆O₁₀ in air at 700?°C.     

硼酸镁过饱和水溶液稀释和酸化过程中的Raman光谱

用纯水和恒沸点盐酸对六硼酸镁过饱和水溶液进行稀释和酸化,使用激光Raman光谱记录反应过程。对光谱峰进行归属。讨论了溶液中含硼量和pH值对硼氧配阴离子存在形式的影响,对多聚硼氧配阴离子在溶液中的存在形式及其相互作用机理进行了初步探讨。     

新型水合稀土多硼酸盐Ln[B5O8(OH)2](Ln=Pr，Nd)的合成与结构

采用熔融硼酸法在200 ℃下合成了一种具有层状结构的新型水合稀土多硼酸盐，Ln[B₅O₈(OH)₂](Ln=Pr，Nd)，并利用粉末X射线衍射技术确定了它的结构。Ln[B₅O₈(OH)₂]晶体属于单斜晶系、P2₁/c空间群，它的基本构建单元(FBB)是由3个BO₄和2个BO₃组成的双三元环，[B₅O₁₂](2Δ+3T)。每一个FBB和邻近的4个FBB通过共用氧原子相连，形成了具有九元环窗口的层状硼酸根基团，稀土离子位于九元环中心附近。CSD：391317。     

层状硼酸铍H2BeB4O8的合成与结构

在硼酸介质中合成了一种新的具有层状结构的多硼酸铍H₂BeB₄O₈,并利用多晶X射线衍射方法确定了晶体结构。H₂BeB₄O₈的空间群为P2₁/n,晶胞参数a=17.7564(2)?,b=4.2948(1)?,c=7.1532(1)?,β=96.8797(9)°。H₂BeB₄O₈的层状结构由双三元环[BeB₄O₁₁]构成,层之间通过垂直于层平面的羟基所形成的氢键连接成三维结构。     

High carbon yield thermoset resin based on phenolic resin,hyperbranched polyborate,and paraformaldehyde

Hyperbranched polyborate (HBPB) is a new hyperbranched polymer with excellent thermal resistance, which can be used to improve the thermal stability, especially carbon yield, of phenolic resin (PR). In the present paper, thermal properties and curing degrees of the blends of PR and HBPB (PR–HBPB blends) are investigated. It is found that the curing degrees of PR–HBPB blends would be decreased, and the decrease of curing degree can be attributed to the improper ratio of phenol groups of HBPB to hydroxymethyl groups of PR. Paraformaldehyde (PFM) is introduced to remedy the deficiency of hydroxymethyl groups in PR–HBPB blends. The curing degrees of PR–HBPB blends are improved and the carbon yields of the blends of PR, HBPB, and PFM (PR–HBPB–PFM blends) can be up to 75–80% at 800°C in nitrogen. PR–HBPB–PFM blends can be explored as novel precursors for carbon materials with excellent properties, ease of preparation and low cost. Copyright © 2010 John Wiley & Sons, Ltd.     

An efficient,environmentally benign,and solvent-free protocol for the synthesis of 4-substituted 1,5-benzodiazepines catalyzed by reusable sulfated polyborate

An efficient and environmentally benign method has been developed for the one-pot solvent-free synthesis of 4-substituted-1,5-benzodiazepines via three-component reaction of o-phenylenediamine, dimedone with a variety of aldehydes catalyzed by sulfated polyborate. The major advantages of the present method are good to excellent yields, shorter reaction time, simple experimental procedure, easy workup, solvent-free reaction condition, recyclability of the catalyst and ability to tolerate a variety of functional groups which gives economical as well as ecological rewards.     

MgO·nB_2O_3-18%MgSO_4-H_2O体系0℃时的热力学非平衡态液固相关系

在MgO·nB2 O3 18%MgSO4 H2 O体系 0℃结晶过程的动力学研究、用物理方法和化学分析确定析出固相的组成和测定固相共饱和点的基础上 ,给出了该体系 0℃时的热力学非平衡态液固相关系图 .该相图存在四个相区 ,分别与H3 BO3 ,MgO·3B2 O3 ·7.5H2 O ,MgO·2B2 O3 ·9H2 O和 2MgO·3B2 O3 ·15H2 O(多水硼镁石 )相对应 .结果表明MgCl2 和MgSO4介质对镁硼酸盐的析出有不同的影响 .