醇和N,N-二甲基乙酰胺分子间相互作用的FTIR光谱研究

The association between alcohols and N,N-dimethylacetamide in carbon tetrachloride was investigated using FTIR spectroscopy at 298 K.The formation constants for 1∶1 and 1∶2 complexes were calculated using the method of Whetsel and Kagarise.The observed 1∶1 complex values were also verified using the method of Nash.The rate of change in C=O bond moment on complexing with alcohols increased with increasing acidity of alcohols.The formation constant and values of free energy change increased with the increase in carbon chain length of alcohols,which suggested that the degree of complex formation varied with the length of the carbon chain of alcohols.     

水溶性铑膦配合物HRh(CO)(TPPTS)_3及其相关体系的~1H-NMR研究

在液体高分辨ＮＭＲ谱仪上, 测定并比较了具有高效烯烃氢甲酰化活性的水溶性铑膦配合物ＨＲｈ（ＣＯ）（ＴＰＰＴＳ）３ 及与此有关的配体ＴＰＰＴＳ和ＯＴＰＰＴＳ分别在Ｄ２Ｏ、混合溶剂Ｄ２Ｏ－ＴＨＦ（ｄ８）－ＣＤ３ＯＤ中的１Ｈ－ＮＭＲ谱图, 并借助１Ｈ－１Ｈ ＣＯＳＹ谱对上述３ 种化合物的１Ｈ－ＮＭＲ谱峰进行了指认; 讨论了影响化学位移和偶合常数的因素, 为水溶性铑膦配合物催化剂的结构与催化性能的关联及新催化剂设计研究提供了基础数据．     

凤尾蕨科植物中倍半萜类成分的研究进展(Ⅱ)(续完)--1H-茚-1-酮类倍半萜的化学合成、化学转化及生物活性

综述了凤尾蕨科植物中分离得到的1H 茚 1 酮类倍半萜的化学合成、化学转化、生物活性以及1 茚酮倍半萜的二聚体化合物和三环1 茚 1 酮倍半萜等方面的研究情况.     

杂多酸引发四氢呋喃开环聚合反应Ⅷ.以1,1,1-三羟甲基丙烷为分子量调节剂

Polyether triol with molecular weight distribution index being 1.3～1.5 was prepared in yield around 50% by tetrahydrofuran polymerization using heteropolyacid-H-3PW12O40 and ethylene oxide as initiator system and 1,1,1-trihydroxymethylenepropane(TMP) as molecular weight controller.The average hydroxyl functionality was estimated by end-group analysis and VPO to be close or equal to 3. The 1H-NMR　spectra showed that about 1/3 hydroxyl of TMP did not react with the propagating chains in the THF polymerization.Each of the unreacted hydroxyl groups of TMP attached to the middle or to the end of a diol chain as a pendent primary hydroxyl group forming the obtained polyether triol. All the hydroxyls of polyether triol were verified to be active enough towards 4,4′-methylene bis(phenyl isocynate) in the preparation of polyurethanes.     

1-氨基乙叉1,1-二膦酸的合成及其阻垢和缓蚀性能

有机多膦酸是一类多齿配体的螯合剂,能与许多金属离子形成稳定的配合物,70年代国内合成了1-羟基乙叉1,1-二膦酸(HEDP),并已应用于水质稳定,金属缓蚀和无氰电镀。Lukevico 用甲腈、三溴化磷和醋酸合成了1-氨基乙叉1,1-二膦酸 CH_3C(NH_2)(P(O)(OH)_2]_2(AEDP)后,又有人用醋酰胺、醋酸酐、亚磷酸或醋酸铵、醋酸酐、亚磷酸以及醋酸铵、醋酰胺、三氧化二磷(P_4O_6)为原料进行了合成,本文报导用尿素、冰醋酸、三氯化磷合成 AEDP 及其阻垢和缓蚀性能.     

The Study of Alcoholysis of 1,2-Thiazetidine-1,1-dioxide with Quantum Chemical Method

The alcoholysis mechanism of 1,2-thiazetidine-1,1-dioxide with methanol, in which the relatively stable product is sulfonate ester, has been investigated by quantum chemical method. Our calculations indicate the reaction for alcoholysis of 1,2-thiazetidine-1,1-dioxide proceeds via two possible mechanisms: concerted and stepwise. In the stepwise mechanism, two possible reaction pathways can be followed while only one possible reaction pathway can be followed in the concerted mechanism.     

Crystal Structure of 1,1-Dichloro-3-Dichloromethyl-1a-3-Dipenyl-1a,2,3,4-Tetrahydro-1H-Azirino[1,2-a][1,5]benzodiazepine (C23H18Cl4N2)

The crystal structure of the title compound, 1,1-dichloro-3-dichloro-3-dichloromethyl-1a,3-diphenyl-1a,2,3,4-tetrahydro-1H-azirino[1,2-a][1,5]benzodiazepine (C23H18Cl4N2, Mr=464.22) was crystallizedin triclinic, space group P1, with cell dimensions a=9.621(7), b=9.694(9), c=12.669(6) , α=107.99(5)°, β=101.42(5)°, γ=69.94(6)°, V=1050.2(4)3, Z=2, Dc=1.468 g/cm3, CuKα(λ=1.5418). F(000)=1816, μ=2.44 mm-1. The structure was solved by direct methods and refined by full-matrix least-squares method, and the final crystallographic discrepancy factor is 0.063 for 2555observed reflections. The molecular backbone is a tricyclic system with the central seven-membered 1,5-diazepine ring in twisted boat-like conformation and cis-fused to both aziridine ring and benzene ring.     

Synthesis, Structure and Biological Activities of 2-（1H- 1,2,3-Benzotriazol-1 -yl ）-1-（ 4- methylphenyl ）-2-（1H-1,2,4-triazol-l-yl）-1-ethanone

The title compound was synthesized and characterized by IR, ^1H NMR, elemental analysis and single crystal X-ray diffraction analysis. Its biological activities were also tested. The results show that the title compound reveals inhibiting activities towards wheat gibberellin, apple ringspot, tomato early blight, peanut cercospora arachidicola and stem wilt of asparagus.     

HPLC-ELSD测定茜芷胶囊中三七皂苷R1、人参皂苷Rg1及Rb1的含量

利用HPLC-ELSD对茜芷胶囊中的活性成分三七皂苷R1、人参皂苷Rg1和Rb1的含量进行测定.三七皂苷R1、人参皂苷Rg1及Rb1分别在0.13~2.60、0.30~6.00、0.38~7.60μg范围内呈现良好的线性关系,平均回收率分别为98.0%(RSD1.7%),97.1%(RSD1.8%),97.0%(RSD1.5%).该方法简便、准确、重现性好,可用于茜芷胶囊的质量控制.     

杂多酸引发甲氢呋喃开环聚合反应——Ⅶ.以1，1，1—三羟甲基丙烷为分子量调节剂

聚氨酯是由硬段和软段组成,其中的软段主要来源于聚醚或聚酯,通过化学交联反应可改变聚氨酯的力学性能,由过氧化物引发或使用小分子的三醇作为扩链剂对聚氨酯的硬段进行化学交联,所得聚氨酯的性能会变坏;而使用环氧丙烷（PO）与四氢呋喃（THF）的共聚醚三醇来制备在软段化学交联的聚氨酯,所得聚氨酯与由PO－THF共聚醚二醇制备的聚氨酯相比,断裂伸长率有轻微的下降,但抗拉强度得取了很大改善,由此可见,通过聚醚多元醇对聚氮酯的软段进行化学交联,有利于改善其力学性能。     

以深度脱铁Fe-YNU-1分子筛为硅源制备Al-YNU-1及其形成机理

主要研究了以哌啶为模板剂,深度脱铁的Fe-YNU-1分子筛为硅源,采用后合成法制备Al-YNU-1分子筛及其形成机理. 通过考察铝含量、水含量、晶化时间和酸处理条件对形成Al-YNU-1分子筛结构的影响规律,发现Al-YNU-1分子筛骨架中的Al含量较以深度脱硼的B-MWW为硅源得到的样品提高了近一倍. 结果表明,Si源中存在大量晶格缺陷位、酸处理脱除Al-MWW层状前驱中大部分模板剂分子与大量骨架Al是形成Al-YNU-1分子筛的必要条件.     

NEW OPTICALLY ACTIVE AROMATIC POLYIMIDES Ⅱ: SYNTHESIS AND PROPERTIES OF OPTICALLY ACTIVE AROMATIC POLYIMIDE BASED ON (R)-(+)-2, 2′-BIS (2-TRIFLUORO-4-AMINOPHENOXY)-1, 1′-BINAPHTHYL*

Optically active (R)-(+)-2, 2' -bis(2 -trifluoro-4 -aminophenoxy)- 1, 1' -binaphthyl was prepared from1, 1'-bi-2-naphthol. The optically active aromatic polyimide was also successfully synthesized. This newpolymer has good solubility, thermal stability etc. Its specific rotation was found to be +174°, and itschiroptical property was also studied.     

色谱保留值参数与灰色模型参数的关系

用数学方法对灰色ＧＭ（１,１）模型与色谱中表述ｋ′和φ关系的Ａ,Ｂ值间的参数关系进行了推导,得出了两者间的函数关系式,从而预测了化合物的出峰位置以及各种混合组分分离分析的可能性,并对实验数据进行了检验,提出了一个获得适当的修正关系式的方法。结果表明：灰色ＧＭ（１,１）模型完全适合于对色谱参数值问题的研究。     

固相自引发基团置换反应制备LiNi1/3Co1/3Mn1/3O2正极材料

自从2001年Ohzuku T和Makimura Y报导LiNi1/3Co1／3Mn1/3O2正极材料以来，其一直被认为是最有可能取代LiCoO2的新型锂离子二次电池正极材料之一。氢氧化物共沉淀法是最常用的一种合成LiNi1/3Co1／3Mn1/3O2材料的方法，通过混合氢氧化物共沉淀法可以获得有着均一分布且具有很高的振实密度的球形LiNi1/3Co1/3Mn1/3O2。     

钛硅沸石中的一种非活性钛物种

Synthesis of the titanium silicalite TS-1 was first reported by Taramasso et al[1]in 1983. TS-1 has received considerable interest during the last decade because of its unique catalytic properties in oxidation reactions involving H2O2 as the oxidant. It is accepted that the extraframework Ti species in TS-1 favor the decomposition of H2O2and should be avoided. But in the present study, it was observed that there was a kind of Ti species inactive in both the oxidation reaction and the decomposition of H2O2.     

手性苯并咪唑铜(Ⅱ)络合物催化合成1,1''''-联-2萘酚

In the past several decades, much attention has been paid to optically active, C2-asymmetric 1,1′-binaphthalene-2,2′-diol and its derivatives because of their application in inducing chirality in asymmetric synthesis[1,2]. Enantiomerically pure 1,1′-binaphthalene-2,2′-diol has been prepared by many methods ranging from the classical resolution via crystallization of the diastereoisomeric salts[3] to asymmetric oxidative coupling[4～6].     

锂离子电池正极材料LixNi1/3Mn1/3Co1/3O2的合成及电化学性能研究

应用以氢氧化物共沉淀为前驱体的高温固相烧结法合成L iN i1/3Mn1/3Co1/3O2正极材料,研究了沉淀温度及烧结过程锂盐投入量对该材料的结构和电化学性能的影响.结果表明,以室温(~20℃)下合成的氢氧化物为前驱体制备的L iN i1/3Mn1/3Co1/3O2具有较好的电化学性能.高温固相烧结会导致部分L iOH损失,因而在合成过程中需加入过量的氢氧化锂,实验表明L i1.08N i1/3Mn1/3Co1/3O2材料的电化学性能最优.     

锂离子电池正极材料LixNi1／3Mn1／3及电化学性能研究CO1／3O2的合成及电化学性能研究

应用以氢氧化物共沉淀为前驱体的高温固相烧结法合成LiNi1/3Mn1/3Co1/3O2正极材料，研究了沉淀温度及烧结过程锂盐投入量对该材料的结构和电化学性能的影响．结果表明，以室温（-20℃）下合成的氢氧化物为前驱体制备的LiNi1/3Mn1/3Co1/3O2具有较好的电化学性能．高温固相烧结会导致部分LiOH损失，因而在合成过程中需加入过量的氢氧化锂，实验表明Li1.08Ni1/3Mn1/3Co1/3O2材料的电化学性能最优．     

1-甲基-1-乙氧基-1-烷硫基甲烷类化合物的合成研究

本文以乙缩醛和烷基硫醇为原料,在30－35℃于四氯化碳中反应20min左右,分别合成1－甲基－1－乙氧基－1－烷硫基甲烷,经红外光谱,质谱以及核磁共振谱检测,确证了产物结构。