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1.
1,2-双(四甲基环戊二烯基)四甲基二硅烷与正丁基锂作用生成(四甲基二硅撑)双(四甲基环戊二烯基负离子盐),后者随即与六碳基钼反应形成1,1'-(四甲基二硅撑)双(四甲基环戊二烯基铝负离子盐)-(Me2SiSiMe2)[Me4CpMo(CO)3-Li+]2(I),I与冰醋酸作用,随即分别与CCl4,NBS及I2反应,生成相应的铝卤化合物(Me2SiSiMe2)[Me4CpMo(CO)3X]2[X=Cl(1),Br(2),I(3)].I与CH3I反应,在钼原子上发生烃基化,得到产物(Me2SiSiMe2)[Me4CpMo(CO)3Me]2(4);I与单质I2直接反应,生成脱硅桥产物Me4Cp(CO)>3I(5).经元素分析、IR及1HNMR表征了化合物1-5的结构。 相似文献
2.
以间氯苯胺与乙氧基亚甲基丙二酸二乙酯(EMME)为原料, 经缩合、 高温环合、 水解、 氯代和亲核取代等反应设计并合成了16个3位为(4'-吗啉)-羰基或乙氧羰基的4-苯氨基喹啉化合物(Ⅰ1~Ⅰ10, Ⅱ1~Ⅱ6). 目标化合物结构经MS及1H NMR确证. 以MTT法, 采用表皮生长因子受体(EGFRs)高表达的人癌细胞(HeLa, HepG2, BGC-823)对目标化合物进行活性测试, 结果表明, 该类化合物对HeLa, HepG2和BGC-823细胞增殖具有一定程度的抑制作用. 其中化合物Ⅱ4~Ⅱ6 对 HepG2 细胞抑制作用较强, 化合物Ⅱ1和Ⅱ5对BGC-823细胞抑制作用较强. 初步探讨了化合物结构与生物活性的关系. 相似文献
3.
碳锗双桥连二环戊二烯(Me2C)(Me2Ge)(C5H4)2(1)与五羰基铁在回流甲苯及二甲苯中的反应,得到正常的Fe-Fe键化合物(Me2C)(Me2Ge)[(η5-C5H3)Fe(CO)]2(μ-CO)2(3)和脱锗桥产物(Me2C)[(η5-C5H4)Fe(CO)]2(μ-CO)2(4)以及一个结构新颖的化合物(Me2C)[(η5-C5H3)[(Me2Ge)Fe(CO)2](η1,η5-C5H3)[Fe(CO)2](2).用X射线衍射分析測定了化合物3的晶体结构,并提出了可能的生成机理. 相似文献
4.
通过1,3-二(1-茚基)四甲基二硅氧烷的双锂盐与TiCl4·2THF反应制得硅桥联二(1-茚基)钛化合物(Me2SiOSiMe2)[Ind]2TiCl2(1),对其催化氢化得到相应的四氢茚基化合物(Me2SiOSiMe2)[IndH4]2TiCl2(2).对化合物1和2的单晶进行了X射线衍射结构分析,它们的晶体都属单斜晶系,P21/n空间群. 相似文献
5.
硅桥连双(三甲硅基环戊二烯基)双锂盐与TiCl4·2THF反应,生成相应的钛化合物[E(C5H3SiMe3)2]TiCl2[E=Me2SiSiMe2(3),Me2SiOSiMe2(5)],同时还分离到了脱一个三甲硅基的产物[E(C5H4)(C5H3SiMe3)]TiCl2[E=Me2SiSiMe2(4),Me2SiOSiMe2(6)].其中四甲基二硅氧桥连配体更容易发生这种脱硅基反应.通过元素分析、MS和1HNMR谱表征了化合物3-6的分子结构. 相似文献
6.
含有酯基及酰胺基柔链的苯并菲盘状液晶的合成、分子间氢键对柱状介晶性的影响 总被引:1,自引:1,他引:0
合成了三个系列, 共二十四个有两种不同软链的对称和非对称苯并菲盘状液晶化合物, C18H6(OR)3- (OCH2COOEt)3, C18H6(OR)3(OCH2COOBu)3, C18H6(OR)3(OCH2CONHBu)3, 其中R=C5H11, C6H13, C7H15, C8H17. 化合物通过柱层析纯化, 结构通过1H NMR, IR, 元素分析等确证. 化合物热稳定性通过TGA测定, 并显示出较高的热稳定性. 通过偏光显微镜和差视扫描量热法对这些化合物的热致液晶性进行了研究. 结果显示: 对于苯并菲液晶化合物C18H6(OR)3(OCH2COOEt)3, 非对称性化合物较之对称异构体化合物有更低的熔点和更高的清亮点, 因而非对称性化合物有更宽的介晶温度范围. 对于分子中含有酰胺基的苯并菲液晶化合物C18H6(OR)3(OCH2CONHBu)3, 对称化合物有比非对称异构体更高的清亮点和更有序的六方柱状介晶相, 且其与具有同样软链长度的分子中不含酰胺基的化合物系列C18H6(OR)3(OCH2COOBu)3相比较, 由于柱内分子间氢键的形成, 不仅有更高的熔点和清亮点, 而且有更丰富的柱状介晶相. 相似文献
7.
含有双胺基的三硅氧烷中的伯胺基与D-葡萄糖酸-δ-内酯进行酰胺化,仲胺基与低聚乙二醇甲醚缩水甘油醚、二缩水甘油醚进行烷基化,制备了新型含硅表面活性剂Me3SiOSiMeR1OSiMe3 [R1=(CH2)3NR2(CH2)2NHCO(CHOH)4CH2OH; R2=H, CH2CH(OH)CH2O(CH2CH2O)xCH3, x=1, 2, 3] (1a, 2a~2c)和(CH2OCH2)y(Me3SiOSiMeR3OSiMe3)2 [R3=(CH2)3NR4~(CH2)2NHCO(CHOH)4CH2OH; R4=CH2CH(OH)CH2OCH2, y=0, 1, 2] (3a~3c).这些化合物的结构用1H, 13C核磁共振仪和元素分析仪进行鉴定.研究了这些新型含硅表面活性剂的界面性能,在浓度分别为10-4和10-5 mol·L-1时可以将水的表面张力降低至约21 mN·m-1. 相似文献
8.
化合物Al2Mo3-xWxO12的合成与结构 总被引:1,自引:0,他引:1
赵新华 《高等学校化学学报》1999,20(3):339-343
合成并表征了一系列化合物Al2Mo3-xWxO12 x=0,0.5,1.0,1.5和2.0的化合物是以单斜晶系Al2(MoO4)3为基质的化合物和固溶体,空间群为P21/a;x=2.5和3.0的标题化合物是以正交晶系Al2(WO4)3为基质的固溶体和化合物,空间群为Pbcn.利用粉末X射线衍射图谱全谱拟合的方法精修了x=0,0.5,1.0,1.5,2.0的标题化合物的结构,讨论其相变机理. 相似文献
9.
在加压固定床反应器上考察了K2CO3、Na2CO3、Ca(OH)2、Ni(NO3)2催化剂对呼和浩特煤加氢气化反应的催化效果,并考察了温度对催化剂效果的影响。实验结果表明,不同种类的金属化合物对气化反应的催化效果有明显影响,催化活性依次为K> Na> Ni> Ca。与原煤气化相比,在相同时间内达到相同碳转化率时,碱金属化合物K2CO3的加入使原煤加氢气化的气化温度降低150℃以上,碱金属化合物Na2CO3降低约150℃,过渡金属化合物Ni(NO3)2降低50℃以上,碱土金属化合物Ca(OH)2的加入会吸收一部分CO2产品,表观上反而降低了碳转化率。SEM及BET表征结果表明,煤样负载不同金属化合物催化剂后表面形态及孔结构有一定差异。 相似文献
10.
分子磁体的设计与合成一直是当今物理和化学的热门研究课题. 受分子磁体启发, 通过引入叠氮磁耦合基团以及长链棒状配体4,4'-二咪唑联苯(L), 我们构筑了三个磁性化合物[Co2(N3)4(L)2.5]∞(1), [Ni2(N3)3(NO3)(L)2.5]∞(2)和[Mn2(N3)4(L)2.5]∞(3). 结构分析显示, 这是三个同构化合物, 展现了一种基于线性叠氮四核单元的二维层网络. 有意义的是, 这种线性叠氮四核单元还未曾被人报道. 磁性研究表明, 三个化合物都是铁磁耦合, 这是由于EO-叠氮所导致的. 通过拟合实验数据, 我们得到了三个化合物的磁耦合常数, 进一步验证了上面磁构相关性的讨论. 相似文献
11.
The drug molecule is called as silα-drug if one carbon atom is substituted by silicon atom in the organic-drugs. Generally, drugs of this kind have low toxicity and pro-long efficiency. People have designed many methods in order to decrease the toxicity of organotin compounds and organosilicon has proved to be effective. Torque[1] is a new acaricide made by Shell company in America, its structure is[(PhMe2CCH2)3SnI2O. R. Tacke[2] from Germany synthesized the compounds (PhMe2SiCH2)3SnX[X=HO, (PhMe2SiCH2)3SnO] and tested the acaricidal activity of[(PhMe2EICH2)3Sn]2O (EI=C, Si) in 1986. He proved that the silyl-derivatives of Torque were highly effective acaricides. 相似文献
12.
Jaime R. Blanton Tianniu Chen Jonathan B. Diminnie Hu Cai Zhongzhi Wu Liting Li Karn R. Sorasaenee Keith T. Quisenberry Hongjun Pan Chang-Sheng Wang Sai-Heung Choi Yun-Dong Wu Zhenyang Lin Ilia A. Guzei Arnold L. Rheingold Ziling Xue 《Journal of molecular catalysis. A, Chemical》2002,190(1-2):101-108
Alkylidene complexes (Me3SiCH2)3Ta(PMe3)=CHSiMe3 (1) and Me3SiCH2Ta(PMe3)2(=CHSiMe3)2 (3a) were found to react with phenylsilanes H2SiR′Ph (R′=Me, Ph) and (PhSiH2)2CH2 to give disilyl-substituted alkylidenes (Me3SiCH2)3Ta=C(SiMe3)(SiHR′Ph) (2) and novel metallasilacyclobutadiene and metalladisilacyclohexadiene complexes. Silyl-substituted alkylidene complex (ButCH2)2W(=O)[=C(But)(SiPh2But)] (5a) was prepared from the reaction of O2 with an equilibrium mixture (ButCH2)W(=CHBut)2(SiPh2But) (4b) (ButCH2)2W(CBut)(SiPh2But) (4a). Our recent studies of the preparation of these complexes and mechanistic pathways in the formation of these silyl-substituted alkylidene complexes are summarized. 相似文献
13.
Amanmammet Bugrayev Nazli Al-Haq Rukeme A. Okopie Asma Qazi Michael Suggate Alice C. Sullivan John R.H. Wilson 《Journal of molecular catalysis. A, Chemical》2008,280(1-2):96-101
New covalently linked sulfonic acid modified silicas have been formed and characterised and their catalytic Brönsted activity evaluated. Thus phenylmercaptoethyltrimethoxysilane, (MeO)3SiCH2CH2SC6H5 and benzylmercaptoethyltrimethoxysilane, (MeO)3SiCH2CH2SCH2C6H5, were used to prepare the corresponding T-functional silica derivatives silica CH2CH2SC6H4-4-SO3H and silica CH2CH2SCH2C6H4-4-SO3H by grafting on commercial silica, followed by sulfonation of the aryl group. Solid-state NMR, DTA and surface area characteristics of the materials are reported. The mercaptophenylsulfonic acid materials are thermally robust highly efficient solid catalysts for a range of transformations including, esterification, etherification and carbonyl group protection. An apparent pore size effect on rate of conversion was observed. The mercaptobenzylsulfonic acid materials were comparatively unstable. 相似文献
14.
四甲基双硅桥联环戊二烯基钠与无水三氯化稀土在THF溶剂中反应合成了标题配合物Me4Si2(C5H4)2LnCl[Ln:3Nd,4Sm,5Gd,6Y]和配合物Me4Si2(C5H4):Ln(C5H5)(THF)n[Ln:1La,n=1;2Pr,n=0].通过元素分析、1HNMR、13CNMR和MS确证了配合物的结构,在THF溶液中重结晶获得配合物4的单晶,x射线衍射证明晶体结构为二聚体,4为单斜晶系,空间群为P21/c,晶体学数据a=1.2982(3)nm,b=1.2269(3)nm,c=1.3681(2)nm,β=96.79(2)°,V=2.162(1)nm3,Z=2,Dx=1.53g/cm3,偏差因子R=0.068. 相似文献
15.
Liliane G. Hubert-Pfalzgraf Nadia Touati Sergej V. Pasko J. Vaissermann Adulfas Abrutis 《Polyhedron》2005,24(18):3066-3073
Hafnium β-diketonatochlorides HfCl2(thd)2 (1), HfCl(thd)3 (2) as well as β-diketonato-silylamide and/or siloxide derivatives of 1 namely Hf(thd)2[N(SiMe3)2]2 (3), Hf(thd)2(OSiMe3)2 (4) and Hf(thd)2(OSitBuMe2)2 (5) (thd = 2,2,6,6-tetramethyl-3,5-heptanedionate) were synthesized and characterized by elemental analysis, FT-IR, 1H NMR and TGA. 2 and 5 were also characterized by single-crystal X-ray diffraction. The siloxide ligands are in cis position for 5 and exert a strong trans effect. The new volatile compounds were tested as single-source precursors for the deposition of HfSixOy films by pulsed liquid injection MOCVD on Si(1 0 0) and R plane sapphire. The as-deposited at 600–800 °C films were essentially amorphous, Hf-rich (Hf/Hf + Si = 0.7–0.85) and smooth. 相似文献
16.
We reported here four structures of lanthanide–amino acid complexes obtained under near physiological pH conditions and their individual formula can be described as [Tb2(dl-Cys)4(H2O)8]Cl2 (1), [Eu4(μ3-OH)4(l-Asp)2(l-HAsp)3(H2O)7] Cl · 11.5H2O (2), [Eu8(l-HVal)16(H2O)32]Cl24 · 12.5H2O (3), and [Tb2(dl-HVal)4(H2O)8]Cl6 · 2H2O (4). These complexes showed diverse structures and have shown potential application in DNA detection. We studied the interactions of the complexes with five single-stranded DNA and found different fluorescence enhancement, binding affinity and binding stoichiometry when the complexes are bound to DNA. 相似文献
17.
Geometrical isomerization of fac-Mo(CO)3L3 (L = P(OPh)3, P(OMe)3, P(OEt)3) to the mer form and that of cis-Mo(CO)4L2 (L = P(OPh)3, P(OMe)3, PPh2(OMe)) to the trans form were observed in CH2Cl2 at room temperature in the presence of a catalytic amount of Me3SiOSO2CF3 (TMSOTf). Crossover experiments suggest that a ligand dissociation is not involved in the isomerization. A catalytic cycle involving an interaction of the silicon atom in Me3Si+ with one oxygen in P(OR)3 ligands has been proposed. The first isolation and the X-ray structure analysis were attained for mer-Mo(CO)3{P(OPh)3}3 through the TSMOTf-assisted isomerization of fac-Mo(CO)3{P(OPh)3}3. 相似文献
18.
采用多种芳香双酯作为电子给予体制备了丙烯聚合高效催化剂,该催化剂具有高活性、聚合反应平稳、产物等规度高等特征.研究了多种芳香双酯和外加各种烷基硅氧烷对丙烯聚合的作用,测定了聚合反应动力学曲线,确定了聚合动力学方程.用扫描电镜研究了催化剂的形态,表明双酯组份能使催化剂结合得较紧密;对聚合产物的结构用DSD、红外光谱进行了表征. 相似文献
19.
Leopoldo Contreras Antonio Pizzano Luis S nchez Ernesto Carmona 《Journal of organometallic chemistry》1995,500(1-2):61-67
The following structural peculiarities of the agostic acyl structure
2R) (R = H, SiMe3) and some characteristic chemical reactivity of the M-η2-acyl and iminoacyl linkage are described. (i) A structural comparison of the bonding parameters within three agostic acetyl Mo complexes containing the dithioacid ligand, indicates that the agostic interaction strengthens upon increasing the electron-releasing properties of the S-chelating ligand. (ii) The acyl-xanthate complex Mo(C(O)Me)(S2COR)(CO)(PMe3)2 undergoes loss of a sulfur atom from the coordinated xanthate and coupling with the acyl ligand to form complexes containing coordinated alkoxythiocarbonyl and monothioacetate ligands. The latter can be metathetically replaced by KS2COR. (iii) Upon heating at 70°C η2-acyl-dicarbonyl bispirazolilborate complexes of molybdenum of the type Mo(H2B(pz*)2)(η2-C(O)Me)(CO)2(PMe3) (pz* = 3,5-dimethyl-pyrazol-1-yl) yield functionalized acyl ligands derived from the stereo- and regioselective intramolecular addition of one of the B---H bonds of the H2B(pz*)2 group across the C=O moiety of the η2-acyl group. (iv) The η2-acyl-isocyanide complexes {Mo}(η2-C(O)R)(CNR′) ({Mo} = Mo(H2B(pz*)2)(CO)(PMe3)) undergo irreversible thermal isomerization to the corresponding η2-iminoacyl-carbonyl derivatives {MO}(η2-C(NR′)R)(CO). This isomerization reaction follows first-order kinetics. 相似文献
20.
When 2-chloro-1,1,1,3,3,3-hexaphenyltrisilane is treated with an excess of HCl in a stainless steel autoclave, two phenyl groups per silicon atom are substituted by Cl yielding 1,1,2,3,3-pentachloro-1,3-diphenyltrisilane. All phenyl groups are replaced upon treatment with HCl/AlCl3 in benzene solution. Coupling of the resulting trisilanes with (tBu)2Hg leads to branched hexasilanes (XCl2Si)2SiClSiCl(SiCl2X)2 (X = Ph, H), which are converted to the corresponding silicon hydrides by LiAlH4. From the reaction of 1,4-diphenyl-2,3-bis(phenylsilyl)tetrasilane with HCl or HBr the tetrahalohexasilanes (ClH2Si)2SiHSiH(SiH2Cl)2 and (BrH2Si)2SiHSiH(SiH2Br)2 can be obtained. 相似文献