Hypervalent Iodine(III) Sulfonate Mediated Synthesis of Imidazo[1,2‐a]pyridines

A direct and efficient method for the conversion of alkyl aryl ketones to imidazo[1,2‐α]pyridines has been developed based on initial formation of α‐organosulfonyloxy ketones and their subsequent cyclocondensation by 2‐aminopyridines in one‐pot conditions.     

Michael Addition of Thiols to á,(a)-Unsaturated Carbonyl Compounds Catalyzed by Bifunctional Organocatalysts:Asymmetric Michael Addition and Asymmetric Protonation

Recently the hydrogen-bond activated reactions have attracted much attention.1 Takemoto2 reported a highly enantioselective Michael addition of manolate to nitroolefins catalyzed by a bifunctional organocatalyst with tertiary amine and thiourea moiety. As we known,stereoselective conjugate additions of thiols are interesting due to the standpoint of biological and synthetic importance, however, only very limited good results have been obtained except for the works of Shibasaki3, Kanemasa4 and Deng5 et al.In this letter, we report an efficient catalytic asymmetric Michael reactions of thiols to a,a-unsaturated carbonyl compounds promoted by bifunctional organocatalysts. A series of organocatalysts with chiral amine and thiourea structures were designed and synthesized and have been successfully applied in the conjugated additions of thiols to a,a-unsaturated imides and enones.The reactions got quantitative yields and the ee values were up to 84%. It is noteworthy that the a-asymmetric protonation (up to 43% ee) also could be achieved.The Michael addition between aromatic thiols and a,a-unsaturated carbonyl compounds isdescribed as follows:Works to further increase the enantioselectivity is under investigation in our laboratory.     

Diastereoselective Three Component Reaction of N‐Glyoxyloyl Camphorpyrazolidinone,Amine and Allyltributylstannane: Facile Synthesis of Homoallylic Amines

Diastereoselective allylation of imine derived from N‐glyoxyloyl camphorpyrazolidinone and amines was treated with allyltributylstannane in the presence of triflic acid. The corresponding optically enriched homoallylic amines were obtained in reasonable to high material yields and with practical levels of stereoselectivity in 10 min at ambient temperature.     

Defect concentration in Ti-substituted YIG from TG curves

The article discusses theory and experiment about the measurement of defect concentration in Ti-substituted yttrium iron garnet by means of thermogravimetry techniques. The two possible cases arising from oxygen interchange with atmosphere, oxygen vacancies and interstitial cations, may be analyzed quantitatively from the derived expressions. The possibility of another type of defects being present in the samples, not associated to oxygen evolution, is not excluded. Measurements were carried out in air and CO₂ for different Ti contents. The substitution tends to increase slightly the defect parameter θ in YIG, while a CO₂ reducing atmosphere is much more effective than the Ti substitution for increasing θ. Calculations for a given single-phased sample sintered in air show two possibilities: a deficit of one oxygen atom for every 2.5 unit cells of 96 atoms, or one excess cation for every 3.5 cells. Other samples show very similar results. The accuracy involved in the measurements is about 2–3%.     

超声条件下溶胶-凝胶法制备CaSiO_3∶(Pb,Mn)发光材料的研究

采用溶胶-凝胶法并辅以超声技术制备了CaSiO3∶(Pb,Mn)发光材料,对合成物运用荧光光谱、DTA-TG、XRD、FTIR、TEM等手段进行了表征。研究了制备时的物料配比、超声时间及焙烧温度对样品发光强度的影响,找到了最佳的合成条件。结果表明,所得样品其荧光强度约为高温固相法样品的2倍,平均粒径则降低约300 nm。     

Interparticle interactions in agglomerates of alpha-Fe2O3 nanoparticles: influence of grinding

We have chemically prepared a sample of antiferromagnetic alpha-Fe2O3 nanoparticles by a gel-sol technique. M?ssbauer spectra of the as-prepared sample showed that superparamagnetic relaxation was suppressed due to strong magnetic interparticle interactions even at room temperature. However, subsequent grinding of the sample by hand in a mortar for some minutes resulted in fast superparamagnetic relaxation of some of the particles. The effect was even more dramatic if the alpha-Fe2O3 powder was ground for a longer time or together with nonmagnetic eta-Al2O3 nanoparticles. Similar effects were found after low-energy ball milling. Thus it is found that the agglomeration of the nanoparticles during preparation under wet conditions results in strong magnetic interparticle interaction, but a relatively gentle mechanical treatment is sufficient to break up the agglomerates, resulting in much weaker interactions. We show that these effects can also be seen when a soil sample containing magnetic nanoparticles is ground.     

CdSe/ZnS-labeled carboxymethyl chitosan as a bioprobe for live cell imaging

A simple and convenient method for the construction of CdSe/ZnS-labeled polysaccharides as bioprobes were developed, which are highly biocompatible and photostable, and have been proven to be suitable for live cell imaging.     

分数导数结合傅里叶最小二乘拟合处理含噪音的重迭信号

提出了一种含噪音重迭信号的综合处理方法 :先用傅里叶最小二乘法拟合噪音数据 ,然后对拟合后的信号求 2 .5次导数 ,在对模拟数据研究的基础上 ,讨论了求导后峰位漂移及其影响因素 ,给出了一个用于矫正峰位值的经验公式。用该方法对模拟和实际的紫外含噪音重迭信号进行处理 ,结果良好     

电动势法测定Cu(Ⅰ)与乙炔生成配合物的热力学函数

乙炔与Cu(I)生成配合物的热力学函数文献报道鲜见,且不同作者的测定结果差异较大。本文用改进的电动势法。对在氯丁橡胶、聚氯乙烯,乙醛等工业过程有重大意义的Cu(I)与乙炔配合物进行测定,得到更合理的结果。