2,6-Lutidine-N-oxide complexes of rare-earth bromides

2,6-Lutidine-N-oxide (LNO) complexes of rare-earth bromides of the composition wheren = l for M = La, Pr, Nd, Sm, Gd, Ho, Er; andn = 0 for M = Y have been prepared and characterised by analyses, conductance and infrared data. Infrared spectra of the complexes indicate that the coordination of ligand to the metal ion takes place through the oxygen of the ligand, and the water molecule in the complexes present is coordinated to the metal. A coordination number of seven has been suggested to all the rare-earth metal ions.     

新型大位阻取代茂钛,锆化合物的合成及其谱学性质

通过１－环庚烯基锂与６，６－二烷基富烯发生环外双键的加成反应形成的大取代茂锂试剂与ＭＣｌ４（Ｍ＝Ｔｉ，Ｚｒ）反应，合成了１２个含或不含手性碳的大位阻取代茂金属有机化合物，并研究了它们的１ＨＮＭＲ，ＥＩＭＳ和ＩＲ．     

1,5-苯并硫氮杂-α-苯基-β-内酰胺的合成及晶体结构

1，5-苯并硫氮杂与苯乙酰氯反应生成1，5-苯并硫氮杂-α-苯基-β-内酰胺（Ⅱ）。X-射线单晶衍射测定结果表明，该化合物分子式为C29H22CINOS，M=467.5，晶体属单斜晶系，P21／c空间群，a＝12．864（3），b=9．511（2），c=19．489（4）A，β=92.41（3）°，V=2382（1）A3，Dc=1．305g／cm3，Z=4，F（000）=976，μ=0．2636mm－1，R=0．068，Rw=0.068。该反应具有立体专一性，四员环上的2个苯基位于同一侧为顺式。产物分子中的七员环为类椅式构象。     

An Efficient Synthesis of <Emphasis Type="Italic">O</Emphasis>-Methyl Protected Emodin Aldehyde and Emodin Nitrile

Summary. An efficient synthesis of tri-O-methylemodin aldehyde was achieved via bromination of tri-O-methylemodin utilizing N-bromosuccinimide yielding the monobromo and dibromo derivatives. Sommelet reaction of the monobromomethyl derivative as well as hydrolysis of the dibromomethyl analog with aqueous silver nitrate afforded the protected aldehyde in good yield. Accordingly, both bromo derivatives can be used even when they are obtained as a mixture of the bromination reaction, which could not be controlled easily to yield the bromo products selectively. From the aldehyde the tri-O-methylemodin nitrile was prepared in a one-pot reaction using hydroxylamine-O-sulfonic acid.Received February 18, 2003; accepted March 3, 2003 Published online June 2, 2003     

Dy(ClO_4)_3·3H_2O-18C6-CH_3CN体系的相平衡及其固体配合物的合成

近年来稀土冠醚配合物的研究受到广泛重视,但稀土高氯酸盐冠醚配合物的研究报道较少。高氯酸镝与冠醚18C6的配合物尚未见报道。我们利用半微量相平衡方法研究了Dy(ClO_4)_3·3H_2O-18C6-CH_3CN三元体系在15℃时的溶解度。同时制得了固态配合物,用化学分析及物理化学方法研究了配合物的组成和性质。     

洋葱色素的提取及抗氧化活性的测定

分别用芬顿（Fenton）反应法和1，1-二苯-2-苦肼基（DPPH）法测定了洋葱色素的抗氧化作用。结果表明，洋葱色素对羟自由基和DPPH自由基均有一定的清除作用，其清除率大小依次为42．4％，58．2％。洋葱色素是十分具有开发利用价值的天然色素。     

Synthesis of new functional derivatives of pyrazolidine from 1-acetyl-3-methyl-5-nitromethyl-2-phenylpyrazolidine

3-Nitromethylpyrazolidine reacts with derivatives of unsaturated acids and reducing agents with the formation of polyfunctional compounds of the pyrazolidine nucleus. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1365–1369, September, 2006.     

绝热法研究己内酰胺阴离子聚合尼龙动力学

采用己内酰胺钠盐、N-75缩二脲作为反应催化体系, 确定反应温度在145-160 ℃之间, 通过计算得到动力学参数: 反应级数为准一级、活化能在73.2-77.1 kJ·mol-1之间、指前因子在2.9×1011-3.6×1011 mol1-n·s-1范围内. 本实验条件下测定并计算的反应热为134.5-137.3 J·g-1, 与文献值(138.6 J·g-1)吻合. 并在前人基础上修正并建构了己内酰胺阴离子绝热反应动力学模型, 对反应过程的模拟结果与实验数据基本吻合, 从而证明了本模型的正确合理.     

一维链状配位聚合物{[Cu(μ-H_2L)(L)Cl](ClO_4)_3}_∞的合成、结构及磁性研究(L=N,N'-双(吡啶基-3-亚甲基)-1,5-二氮环辛烷)

设计合成了一个新型吡啶基二氮环配体L(N,N'-双(吡啶基-3-亚甲基)-1,5-二氮环辛烷)及其铜配位聚合物{[Cu(滋-H2L)(L)Cl](ClO4)3}∞(1),研究了此配合物的晶体结构、光谱及磁性质。该配合物属正交晶系,Pnma空间群,晶胞参数为a=3.5170(17)nm,b=1.0440(5)nm,c=1.1966(6)nm,V=4.394(4)nm3,Z=4。配体L以顺式螯合和反式桥联两种不同的配位形式将铜离子连接起来形成一维链状阳离子结构。