Asymmetric reduction of representative ketones with a bis-chiral oxazaborolidine system

In recent years, many optically active β-amino alcohols, mostly derived from naturally occurring α-amino acids, have been incorporated into the asymmetric synthesis as chiral auxiliaries or ligands.1 An effective asymmetric catalysts, the oxazaborolidine-borane reagents, which were originally pioneered by Itsuno and Corey,2 were generally prepared from chiral β-amino alcohols by the reaction with boric acid or formed in situ in the presence of borane. These reagents provide excellent enanti…     

[C6N2H18]2[Mo5O15(HPO4)2]·H2O的水热合成与结构表征

通过水热法合成了一个新化合物[C6N2H18]2[Mo5O15(HPO4)2]·H2O,并通过IR光谱、ICP、元素分析、差热与热重分析和X射线单晶衍射分析等手段进行了表征.结果表明,晶体属三方晶系,P3(2)21空间群,a=1.1231(1)nm,c=2.2802(5)nm,V=2.4911(7)nm3,Dx=2.835Mg/m3,Z=6,最后的一致性因子R=0.0227,wR=0.0675.阴离子中Mo5O15构成一环状结构,2个HPO4一个连在环的下方,一个连在环的上方,形成类似于“飞碟”状的结构,阳离子为2个质子化的四甲基乙二胺.     

再谈磷的同素异形体(1)——块体磷的同素异形体

结合最新研究进展，全面介绍了块体状磷的同素异形体——白磷、红磷、黑磷等，包括存在、组成、性质、结构、制备、应用等，同时明确了紫磷、希拖夫磷、灰磷、褐磷等概念，提出了大学本科化学教学的建议。     

Synthesis and Crystal Structure of[Fe_2V (μ_3-O) (μ-O_2CCH_3)_6 (THF)_3]Cl· 3H_2O

lmTR0DUCTI0NTrivanadium(III)ox0-carb0xylat0complexeshaveattractedmuchinterestre-cently"~".Manyc0mp0unds0fthiskindhavebeensynthesizedandtheirstructural,physicalandspectr0sc0picpr0pertieshavebeenstudied.Butnone0fthiskindofcom-plexeswithmixedmeta1shavebeensynthesized.Hereinwereportthecrystalstruc-tureofthefirstmixedmeta1carboxylatocomp0undofvanadium.2EXPERIMENTAL2.1Synthesis0.l6g(lmmol)VCl3,0.32g(2mmol)FeCl3and0.48g(6mm0l)NaCO,CH,wasdisso1vedinaso1uti0n0ft0luerie(20ml),THF(lOml),ac…     

N，N，N′，N′-四丁基丙二酰胺从硝酸盐介质中萃取铈(Ⅲ)

Study on the extraction and separation of rare earth with new extractants is important in the rare earth chemistry and nuclear reprocessing. In this work， the extraction of Ce(Ⅲ) with N，N，N′，N′-tetrabutylmalonamide (TBMA) in toluene from nitrate media has been investigated. The effect of the concentration of nitric acid， TBMA and salt-ing-out agent (LiNO₃) and also the temperature on the distribution ratios was examined. The stoichiometries of the extracted complexes were determined to be Ce(NO₃)₃·3TBMA and Ce(NO₃)₃·4TBMA， respectively. The ap-parent extraction constants and the enthalpy of the extraction were calculated based on the extraction data， which are logK_ex1=3.97， logK_ex2=4.75 and Δ_rH_m^?=-31.25kJ·mol^-1， respectively. The IR spectra of the loaded organic phase supported the suggested extraction mechanism.     

Novel Water Soluble Fluorescent Trimethine Indocyanines Containing N-ρ-Carboxybenzyl Group

Indocyanine dyes as fluorescent labeling reagents have been used in bioanalysis1,2. Arylsulfonate indocyanine dyes 1d and 1e developed by Waggoner A. S. et al.3,4 have excellent fluorescent properties combined with good aqueous solubility, are a new generation of fluorescent label compounds for proteins, oligonucleotides and other compounds containing hydroxyl, mercaptol or primary amine groups5. However, photostability of these dyes has been a problem. Z. G. YAO et al.6 reported that p…     

侧边抛磨光纤波导传输特性的理论分析

在建立侧边抛磨光纤D型光纤边界条件的基础上,用三维有限差分光束传输法计算和分析了侧边抛磨光纤器件的光功率衰减随光纤的侧边抛磨长度、光纤侧边抛磨后剩余包层的厚度、以及填充聚合物材料折射率三个参量变化的特性.结果表明,侧边抛磨光纤器件的光功率衰减随着抛磨长度的增加而增大;当抛磨长度等于9 mm时,光功率衰减随着剩余包层厚度的增大而单调递减.而当抛磨长度大于9 mm时,剩余包层厚度小于3 μm的范围内,光衰减随着剩余包层厚度的增加出现振荡;当聚合物折射率与纤芯折射率相同时,光功率衰减最大.     

高温高压下β相硼的电导率测量

 硼在高压下具有复杂的结构和多样的物理性质,对其结构和性质的深入研究具有很重要的意义,一直引起理论和实验研究领域的关注。高压下进行电学性质测量是获得物质物理性质的有效手段,利用集成在金刚石对顶砧上的微电路,在高压下和两个不同温度范围内对β相硼进行了电导率测量,分析了导电机制随压力的变化规律。在0～28.1 GPa范围内,β相硼的电导率随着压力的增大是逐渐增大的,卸压后样品的电导率不能回到最初的状态,是一个不可逆的变化过程;由室温到423 K的范围内,β硼的电导率随着温度的不断增加有明显的上升趋势,并且随着压力的升高,电导率变化逐渐加快。此外,对样品在14.5 GPa和18.6 GPa压力下,用溅射到金刚石对顶砧上的氧化铝薄膜做绝热层,对样品进行了激光加热实验,最高温度达到2 224 K,电导率随着温度的上升而增大,结果显示,β相硼的电学特征仍然属于半导体的特征范围内。     

离子交换树脂相分光光度法测定水中痕量铋

利用离子交换树脂相通过光度法测定痕量铋。铋离子在碱性介质中与邻苯二酚紫形成紫色络合物将其富集在苯乙烯阴离子交换树脂上,通过制作成薄层直接光度法测定。本法操作简便,装皿容易,选择性好,精密度高(测定5μgBi3 5次,RSD=3.8%),铋浓度在0~10μg(50ml)时与吸光度呈线性关系,线性回归方程为A=0.010 0.075C(μg/50ml),相关系数r=0.9997,铋的回收率为98%~99%,检出限为3.2μg/L,用于水中痕量铋的测定,结果满意。     

冲击加载条件下材料之间摩擦系数的确定

尝试利用自制分离式霍普金森压剪装置对聚氨酯泡沫塑料、硅橡胶和MDF水泥材料与铝合金在冲击加载条件下的摩擦系数进行测试.结果表明:在冲击加载条件下,聚氨酯泡沫塑料、硅橡胶和MDF水泥与铝杆之间的摩擦系数与材料的性质关系不大,其摩擦系数测试结果存在一定的分散性,摩擦曲线出现抖动,且与加载条件有关,摩擦系数比通常意义下所得到的摩擦系数小;不同加载条件对所测试材料与铝压杆之间的摩擦系数数值影响不大,只是曲线的走势稍有不同.在冲击加载条件下硬质聚氨酯泡沫塑料与铝杆之间的静摩擦系数为0.29,动摩擦系数为0.25;硅橡胶与铝杆之间的静摩擦系数为0.285,动摩擦系数为0.24;MDF水泥与铝合金杆之间的静摩擦系数为0.28～0.29,动摩擦系数约0.23.