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10种二茂铁基-1,1'-二烷基二茂铁经LiAlH4还原得到10种相应的二茂铁基-1,1'-二烷基二茂铁甲醇。这类羟基化合物对酸的敏感性很高。由2种二茂铁基-1,1'-二乙基二茂铁甲醇与BF3在二氯甲烷中反应形成了稳定的二茂铁基-1,1'-二乙基二茂铁甲碳正离子。无需从反应混合中分离,该离子与乙胺作用得到了2种N-取代产物。由元素分析、红外光谱和核磁共振氢谱证实了化合物的结构。 相似文献
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用2-二茂铁基-1,3-二噻烷的锂代物与芳基羰基化合物的反应,合成了16种2-二茂铁基-2-(芳基羟甲基)-1,3-二噻烷.简要讨论了产物的1HNMR谱以及羰基化合物结构对反应的影响. 相似文献
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3-烷基/芳基-6-(1'-N-β-D-或-α-L-吡喃型全乙酰化糖基)- 均三唑并[3,4-b]-1,3,4-噻二唑的合成 总被引:5,自引:0,他引:5
通过2,3,4,6-四-O-乙酰基-β-D-吡喃型葡萄糖异硫氰酸酯(3)和2,3,4-三-O-乙酰基-α-L-吡喃型鼠李糖异硫氰酸酯(4)与3-烷基/芳基-4-氨基-5-巯基-1,2,4-三唑(5)在乙醇中回流,缩合得到了14个新的3-烷基/芳基-6-(1'-N-2',3',4',6'-四-O-乙酰基-β-D-吡喃型葡萄糖基或2',3',4'-三-O-乙酰基-α-L-吡喃型鼠李糖基)-均三唑并[3,4-b]-1,3,4-噻二唑类化合物(6a-6i,7a-7e),化合物结构经元素分析、IR和1H NMR确证. 相似文献
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甲酰基二茂铁是一种极为重要的二茂铁衍生物。以它为中间体 ,经缩合、还原和氧化等反应 [1~ 3] ,可得到许多其它的二茂铁化合物。在甲酰基二茂铁分子中引入烷基后 ,其性质在两个方面会发生显著变化。一是含碳量增加 ,导致其衍生物在有机溶剂中的溶解度增加 ;另一是化合物的物态发生了很大变化 ,固态会变为液态 ,高熔点物会变为低熔点物 ,为合成液态或低熔点二茂铁化合物提供了丰富的中间体。有关二烷基二茂铁甲酰化反应的报道甚少[4 ] ,更未见系统地研究过多种不同烷基的引入对甲酰化反应的影响。为此我们研究了 6种二烷基二茂铁的 Vilsme… 相似文献
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Ratajczak等研究了S-(1-二茂铁烷基)疏代乙醇酸的合成与反应Ugi等将它们与羟胺反应,合成了一种有用的手性模板试剂。最近,Czech等用键合载体液相色谱对它们进行了光学拆分研究。本文报导了此类化合物与胺的反应,合成了一类新的化合物-S-(1-二茂铁烷基)硫代乙醇酸胺。 相似文献
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以二茂铁为原料, 通过合成1,1'-二乙酰基二茂铁、1,1'-二茂铁二甲酸、1,1'-二茂铁二甲酰氯, 在高度稀释条件下与4种二羟乙基苯胺进行酯化反应得到了1,9-二羰基-2,8-二氧-5-(4-氟)苯基氮[9]二茂铁酯环蕃a, 1,9-二羰基-2,8-二氧-5-(4-甲基)苯基氮[9]二茂铁酯环蕃b, 1,9-二羰基-2,8-二氧-5-(4-甲氧基)苯基氮[9]二茂铁酯环蕃c, 1,9-二羰基-2,8-二氧-5-(4-硝基)苯基氮[9]二茂铁酯环蕃d. 用UV、1H NMR、FT-IR、元素分析和基质辅助激光解析电离-飞行时间质谱(MALDI-TOF)对这些化合物进行了表征. 培养了二茂铁酯环蕃a的单晶, 并对其结构进行了解析. 相似文献
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《Journal of Coordination Chemistry》2012,65(10):1664-1675
Three coordination polymers, {[Co(C10H5N3O5)(H2O)2]·H2O}n (1), {[Mn3(C10H5N3O5)2Cl2(H2O)6]·2H2O}n (2), and {[Cu3(C10H4N3O5)2(H2O)3]·4H2O}n (3), based on a T-shaped tripodal ligand 4-(4,5-dicarboxy-1H-imidazol-2-yl)pyridine 1-oxide (H3DCImPyO), were synthesized under hydrothermal conditions. The polymers showed diverse coordination modes, being characterized by elemental analysis, infrared spectroscopy, and single-crystal X-ray structure analysis. In 1, the HDCImPyO2? generated a 1-D chain by adopting a μ2-kN, O : kN′, O′ coordination mode to bridge two Co(II) ions in two bis-N,O-chelating modes. In 2, the HDCImPyO2? adopted a μ3-kN, O : kO′, O′′ : O′′′ coordination mode to bridge two crystallographically independent Mn(II) ions, forming a 2-D hcb network with {63} topology. In 3, by adopting μ4-kN, O : kO′, O′′ : kN′′, O′′′ : O′′′′ coordination, DCImPyO3? bridged three crystallographically independent Cu(II) ions to form a 3-D framework having the stb topology. 相似文献
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Jinglai Zhang Yonghong Li Junfeng Li Xing Chen Zexing Cao 《International journal of quantum chemistry》2009,109(5):1116-1126
The density functional theory (DFT) and the complete active space self‐consistent‐field (CASSCF) method have been used for full geometry optimization of carbon chains C2nH+ (n = 1–5) in their ground states and selected excited states, respectively. Calculations show that C2nH+ (n = 1–5) have stable linear structures with the ground state of X3Π for C2H+ or X3Σ? for other species. The excited‐state properties of C2nH+ have been investigated by the multiconfigurational second‐order perturbation theory (CASPT2), and predicted vertical excitation energies show good agreement with the available experimental values. On the basis of our calculations, the unsolved observed bands in previous experiments have been interpreted. CASSCF/CASPT2 calculations also have been used to explore the vertical emission energy of selected low‐lying states in C2nH+ (n = 1–5). Present results indicate that the predicted vertical excitation and emission energies of C2nH+ have similar size dependences, and they gradually decrease as the chain size increases. © 2008 Wiley Periodicals, Inc. Int J Quantum Chem, 2009 相似文献
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Ludwig Maier 《Helvetica chimica acta》1969,52(3):845-857
Bis-chloromethyl-alkyl-and - aryl-phosphine oxides, (CICH2)2P(O)R, which are obtained by reaction of (CICH2)2P(O)Cl with GRIGNARD reagents, undergo a MICHAELIS -ARBUSOV reaction when heated for several hours with trivalent phosphorus esters (phosphites, phosphonites, or phosphinites) at 170–180°C. The reaction affords bis-(dialkyloxyphosphonyl-methyl)-, bis (alkyloxyphosphinyl-methyl)-, and bis-(oxophosphoranyl-methyl)-, -alkyl- or -aryl-phosphine oxides, R(O)P[CH2P(O)R′R″]2 R = CH3, C2H5, n-C8H17, n-C12H25, C6H5; R′ and R″ = C2H5O, C4H9O, C6H5, CH3 in good yields. Conversion of the compounds containing alkyloxy groups to the free acids is achieved by refluxing with conc. HCl. Bis-(dihydroxyphosphonyl-methyl)-dodecylphosphine oxide, n-C12H25(O)P[CH2P(O) (OH)2]2, obtained by hydrolysis of the all-ethyl ester, titrates in aqueous solution as a tetrabasic acid with breaks at pH = 4 (two equivalents), pH = 6,9 (one equivalent) and pH = 9,6 (one equivalent). This acid, its disodium salt (m. p. 405–410°) and its tetrasodium salt (m.p. > 460°) are surface active and are excellent chelating agents. The 1H- and 31P-NMR. spectra of all the compounds prepared are discussed. 相似文献
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Marcin Rojkiewicz Piotr Ku Maria Ksiek Joachim Kusz 《Acta Crystallographica. Section C, Structural Chemistry》2022,78(1):56-62
Cathinones belong to a group of compounds of great interest in the new psychoactive substances (NPS) market. Constant changes to the chemical structure made by the producers of these compounds require a quick reaction from analytical laboratories in ascertaining their characteristics. In this article, three cathinone derivatives were characterized by X-ray crystallography. The investigated compounds were confirmed as: 1-[1-(4-methylphenyl)-1-oxohexan-2-yl]pyrrolidin-1-ium chloride ( 1 , C17H26NO+·Cl?, the hydrochloride of 4-MPHP), 1-(4-methyl-1-oxo-1-phenylpentan-2-yl)pyrrolidin-1-ium chloride ( 2 ; C16H24NO+·Cl?, the hydrochloride of α-PiHP) and methyl[1-(4-methylphenyl)-1-oxopentan-2-yl]azanium chloride ( 3 ; C13H20NO+·Cl?, the hydrochloride of 4-MPD). All the salts crystallize in a monoclinic space group: 1 and 2 in P21/c, and 3 in P21/n. To the best of our knowledge, this study provides the first detailed and comprehensive crystallographic data on salts 1 – 3 . 相似文献
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The 12.1 eV, 75°C electron impact mass spectra of 24 urethanes, RNHCO2C2H5 [R ? H, C2H2n +1 (n = 1-8), CH2?CHCH2, Ph, PhCH2 and PhCH2CH2], and seven symmetrically disubstituted urethanes R2NCO2C2H5 (R ? Cn H2n + 1 (n = 1?4)) are reported and discussed. All 31 spectra show appreciable molecular ion peaks. For n ?Cn H2n +1 NHCO2C2H5, M+ ˙ usually is the most abundant ion in the spectrum. A peak at m/z 102 of comparable intensity also is present; this corresponds to formal cleavage of the bond connecting the α- and β-carbon atoms in the N-alkyl group, though it is unlikely that the daughter ion has the structure [CH2?NHCO2C2H5]+. In the RNHCO2C2H5 series, branching at the α-carbon atom enhances the relative abundance of the ion arising by notional α-cleavage at the expense of that of M+ ˙. Formal cleavage of the bond between β- and γ-carbon atoms occurs to some extent for [RNHCO2C2H5]+˙ ions; this reaction provides information on the degree of branching at the β-carbon, especially if metastable molecular ions are considered. The higher n-CnH2n +1NHCO2C2H5 (n = 5?8) urethanes exhibit two other significant ions in their mass spectra. First, there is a peak at [M ? C2H5]+. Secondly, a peak is present at m/z 90; the most plausible structure for this ion is [H2N(HO)COC2H5]+, arising by double hydrogen transfer from the alkyl group and expulsion of a [CnH2n ?1]˙ radical. Ions originating from secondary decomposition of the primary ionic species are generally of only very low abundance in these spectra. 相似文献
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The synthesis of 7′-aryl-7′-apo-β-carotenes, where aryl (Ar) is Ph, 4-NO2C6H4, 4-MeOC6H4, 4-(MeO2C)C6H4, C6F5, and 2,4,6-Me3C6H2, is described. NMR Chemical shifts of all H- and C-atoms are presented, together with specific examples of the spectra. In contrast to 1H chemical shifts which, except for H? C(8′) and H? C(7′), did not differ greatly from those of β,β-carotene, considerable variations in 13C chemical shifts were observed. Signals of the C(α) atoms of the polyene chain [C(β)? C(α)] +n Ar were shielded, those of the C(β) atoms were deshielded, with some exceptions when n = 1; the effects decreased with increasing n. 相似文献
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Dr. Yongguang Li Dr. Le Zhao Dr. Anthony Yiu‐Yan Tam Dr. Keith Man‐Chung Wong Prof. Dr. Lixin Wu Prof. Dr. Vivian Wing‐Wah Yam 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(43):14496-14505
A new series of platinum(II) complexes with tridentate ligands 2,6‐bis(1‐alkyl‐1,2,3‐triazol‐4‐yl)pyridine and 2,6‐bis(1‐aryl‐1,2,3‐triazol‐4‐yl)pyridine (N7R), [Pt(N7R)Cl]X ( 1 – 7 ) and [Pt(N7R)(C?CR′)]X ( 8 – 17 ; R=n‐C4H9, n‐C8H17, n‐C12H25, n‐C14H29, n‐C18H37, C6H5, and CH2‐C6H5; R′=C6H5, C6H4‐CH3‐p, C6H4‐CF3‐p, C6H4‐N(CH3)2‐p, and cholesteryl 2‐propyn‐1‐yl carbonate; X=OTf?, PF6?, and Cl?), has been synthesized and characterized. Their electrochemical and photophysical properties have also been studied. Two amphiphilic platinum(II)? 2,6‐bis(1‐dodecyl‐1,2,3‐triazol‐4‐yl)pyridine complexes ( 3‐Cl and 8 ) were found to form stable and reproducible Langmuir–Blodgett (LB) films at the air/water interface. These LB films were characterized by the study of their surface‐pressure–molecular‐area (π–A) isotherms, XRD, and IR and polarized‐IR spectroscopy. 相似文献
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The ring-substituted bis(cyclopentadienyl)silanesMe
2Si(C5H5) (MeC5H4) (1a) andMe
2Si(MeC5H4)2 (2a) could be prepared by the reactions ofMe
2SiCl2 with C5H5Na andMeC5H4Na or only withMeC5H4Na, respectively. Metallation of1 a or2 a withn-BuLi and following reaction with TiCl4 led to the first ringsubstituted [1]titanocenophanes,Me
2Si(C5H4) (MeC5H3)TiCl2 (1 b) orMe
2Si(MeC5H3)2 TiCl2 (2 b), respectively. On reaction with NaI,1 b yieldedMe
2Si(C5H4) (MeC5H3)TiI2 (1 c). Structural assignments of the compounds could be made on the basis of their1H NMR spectra. 相似文献
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Synthesis and Structure of 1—Cyclopentylindenyl Lanthanide(Ⅱ)Complexes and Their Catalytic Behavior for Polymerization of Acrylonitrile 总被引:1,自引:0,他引:1
The reaction between K(1‐C5H9C9H6) and anhydrous LnCl3 (Ln=Sm, Yb) in the molar ratio of 2:1 in THF with subsequent treatment by Na‐K alloy afforded (1‐C5H9C9H6)2Ln‐(THF)n(Ln=Sm, n=1; Ln=Yb, n=2), while the reaction of Sml2 with K(1‐C5H9C9H6) in the molar ratio of 1:2 in THF gave the anionic complex K(1‐C5H9C9H6)3Sm(THF)3. The X‐ray structure of (1‐C5H9C9H6)2Yb(THF)2 showed that central metal Yb is coordinated by two cyclopentadienyl rings of 1‐cyclopentylindenyls and two oxygen atoms from two tetrahydrofuran molecules to form pseudo‐tetrahedral coordinate geometry. All these complexes are active for the polymerization of acrylonitrile. 相似文献
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Run‐Chang Liu Yong‐Qiang Ma Lin Yu Jin‐Shan Li Jing‐Rong Cui Rui‐Qing Wang 《应用有机金属化学》2003,17(9):662-668
A series of arylantimony ferrocenecarboxylates with the formula (C5H5FeC5H4CO2)nSbAr(5?n) (n = 1, 2; Ar = C6H5, 4‐CH3C6H4, 3‐CH3C6H4, 2‐CH3C6H4, 4‐ClC6H4, 4‐FC6H4) were synthesized and characterized by elemental analysis, IR, 1H NMR and mass spectra. The crystal structures of (C5H5FeC5H4CO2)2Sb(4‐CH3C6H4)3 and C5H5FeC5H4CO2SbPh4 were determined by X‐ray diffraction. Four human neoplastic cell lines (HL‐60, Bel‐7402, KB and Hela) were used to screen these compounds. The results indicate that these compounds at 10 µM show certain in vitro antitumor activities. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献