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1.
Three monomeric germatranes, 1-isopropoxy-3,3,7,7,10,10-hexamethyl-2,8,9-trioxa-5-aza-1-germatricyclo[3.3.3.01,5]undecane (1), 1-isopropoxy-3,3,7,7-tetramethyl-2,8,9-trioxa-5-aza-1-germatricyclo[3.3.3.01,5]undecane (2), and 1-isopropoxy-3,3-dimethyl-2,8,9-trioxa-5-aza-1-germatricyclo[3.3.3.01,5]undecane (3) have been synthesized by the reaction of Ge(O-i-Pr)4 in refluxing toluene with corresponding triethanolamines, (HOCH2CH2)nN(CH2CMe2OH)3−n (n = 0, L1H3; n = 1, L2H3; n = 2, L3H3), where the number of CMe2 groups adjacent to a OH functionality varied from 3 (L1H3) to 2 (L2H3), and to 1 (L3H3). These germatranes 1-3 have been characterized by solution 1H and 13C{1H} NMR and the solid state structure of 2 has been determined by single crystal X-ray diffraction.  相似文献   

2.
通过1-(3-氨基丙基)-2,8,9-三氧杂-5-氮杂-1-硅杂双环[3,3,3]十一烷与酸反应或1-(3-氯丙基)-2,8,9-三氧杂-5-氮杂-1-硅杂双环[3,3,3]十一烷与胺反应,合成了14种1-(3-氨基丙基)-2,8,9-三氧杂-5-氮杂-1-硅杂双环[3,3,3]十一烷衍生物.体外细胞培养试验结果表明,某些1-(3-氨基丙基)-2,8,9-三氧杂-5-氮杂-1-硅杂双环[3,3,3]十一烷衍生物对艾氏腹水癌细胞具有较好的杀伤活性.  相似文献   

3.
Enantiospecific synthesis of the tricyclic core structure present in the biologically active natural products tricycloillicinone, ialibinones, and takaneones, starting from the readily available campholenaldehyde employing a transannular RCM reaction as the key step, has been accomplished.  相似文献   

4.
Two new compounds, bis (DL-erythro-α-2-piperydylium-2,8-bis(trifluoromethyl)-4-quinolinemethanol) tetrachlorocuprate(II) tetrahydrate [LH+]2[CuCl4]2??4H2O 1 [L = mefloquine] and bis(DL-erythro-α-2-piperydylium-2,8-bis(trifluoromethyl)-4-quinolinemethanol) tetrabromocadmate (II) bis(methanol) [LH+]2[CdBr4]2?·2CH3OH 2, have been synthesized and characterized by elemental analysis, 1H-NMR and IR spectroscopy. Single-crystal X-ray diffraction analysis of 1 showed the structure to be ionic with formula unit comprising two protonated monocationic mefloquine molecules of opposite chirality, a tetrachlorocuprate (II) anion and a complement of four water molecules, disordered over several sites. The crystals are orthorhombic, space group Pnma, a = 9.6975(1) Å, b = 29.5385(3) Å, c = 15.9423(1) Å, V = 4566.67(7) Å3, Z = 4. The formula unit of compound 2 comprises two protonated monocationic mefloquine molecules, a tetrabromocadmate(II) anion and two molecules of methanol. The crystals are orthorhombic, space group Fdd2, a = 17.2185(5) Å, b = 55.456(2) Å, c = 9.5140(3) Å, V = 9084.6(5) Å3, Z = 8. The mefloquine molecule is protonated at the piperidinyl N atom and extensive hydrogen bonding occurs in both crystal structures. The conformation of the mefloquine cation in 1 and 2 is very similar to that recently observed in other salts of the drug, confirming its relevance in the context of antimalarial action.  相似文献   

5.
The N-ferrocenoyl amino acid ester derivatives FcCOR {Fc=(η5-C5H5)Fe(η5-C5H4)} where R=Gly(OMe) 1, Gly(OEt) 2, Gly(OBn) 3, l-Ala(OMe) 4, l-Ala(OEt) 5, l-Leu(OMe) 6, l-Leu(OEt) 7, l-Leu(OBn) 8, l-Phe(OMe) 9 and l-Phe(OEt) 10, were prepared by coupling ferrocene carboxylic acid with the appropriate amino acid ester starting materials using the 1,3-dicyclohexylcarbodiimide (DCC), 1-hydroxybenzotriazole (HOBt) protocol and these have been characterised by spectroscopic techniques. The electrochemical anion sensing behaviour of compounds 1-10 with several anions using a platinum microdisk working electrode is described, together with 1H NMR anion complexation studies. The X-ray single crystal structure of N-ferrocenoyl-l-alanine methyl ester 4 has been determined and contains two molecules which differ slightly in conformation in the asymmetric unit of space group P21 (No. 4); principal dimensions are amide N(H)CO 1.224(6) and 1.231(6) Å, ester CO 1.220(10) and 1.190(7) Å, with N-H?OC(amide) as the primary intermolecular hydrogen bond, N?O 2.992(6) and 2.971(6) Å and with graph set C(4).  相似文献   

6.
The [{Pr(NO3)2(H2O)3}{Pr(NO3)(H2O)4} (C36H36N24O12)](NO3)3·4H2O and [{Nd(NO3)(H2O)4} 2(NO3@C36H36N24O12)][Nd(NO3)6] complexes were prepared by heating a mixture of lanthanide nitrates, cucurbit[6]uril, and water in a sealed tube. X-ray diffraction study demonstrated that the metal atoms in the former complex are linked to the macrocycle through tridentate coordination of the portal oxygen atoms of cucurbit[6]uril to the praseodymium(III) cation. The neodymium(III) complex is the first example of lanthanide compounds with cucurbit[6]uril belonging to coordination polymers. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1511–1517, September, 2006.  相似文献   

7.
The pyrazinium salt [FcCH2pyz][BF4] (1) and the quinoxalinium salt [FcCH2quin][BF4] (2) were prepared by the reaction of [FcCH2][BF4] with pyrazine and quinoxaline, respectively and characterised by spectroscopic methods, cyclic voltammetry and by single-crystal X-ray diffraction, which revealed the absence of any π-π-stacking motifs in the crystal structures.  相似文献   

8.
In situ 1H nuclear magnetic resonance spectroscopy was used to investigate the processes that occur during the synthesis of 1,3,6,8-tetraazatricyclo[4.3.1.13,8]undecane (TATU). NMR analysis showed a reaction mixture containing more than one compound. The production of these intermediates and collateral products was rationally supported by a careful 1H NMR monitoring study. We characterized 1,3,5-triazabicyclo[3.2.1]octane (TABO, 4) and 3-(2-aminoethyl)-1,3,5-triazabicyclo[3.2.1]octane (AETABO, 7) by 1H and 13C NMR in D2O solution inside the NMR sample tube, as an intermediate and collateral product of the reaction, respectively. Further, a reaction of 1,3,6,8-tetraazatricyclo[4.4.1.13,8]dodecane (TATD) with 15N-labeled ammonium chloride was carried out. The 15N NMR and GC-MS experiments indicated that 15N was incorporated into TATU, TABO, and urotropine.  相似文献   

9.
Fluorotitanates (LH)2[TiF6nH2O (1: R = pyridine, n = 1, 2: R = 2-picoline, n = 2, 3: R = 2,6-lutidine, n = 0, 4: R = 2,4,6-collidine, n = 0) and (LH)[TiF5(H2O)] (3a: L = 2,6-lutidine) have been synthesized by the reaction of pyridine or corresponding methyl substituted pyridines and titanium dioxide dissolved in hydrofluoric acid. The crystal structures of ionic compounds 1, 2, 3, 3a and 4 have been determined by single-crystal X-ray diffraction analysis. The hydrogen bonding led to the formation of discrete (LH)2[TiF6] units (4), chains (1-3), and layers (3a). The additional π-π interactions present in 1, 2, and 4 results in chain structures of 1 and 4 and in a layer structure of 2. The [TiF6]2− and [TiF5(H2O)] anions were observed by 19F NMR spectroscopy in aqueous solutions of 1, 2, 3, 3a and 4.  相似文献   

10.
An efficient method for the synthesis of some difunctionalized copillar[5]arene Schiff bases from condensation of salicylaldehyde and its 5-chloro, 5-bromo, 3,5-di(t-butyl) substituted derivatives with corresponding diamino-functionalized copillar[5]arene, which were prepared by Gabriel reaction according to the reported method. Single-crystals of six copillar[5]arenes were determined by X-ray diffraction. An ORTEP of compounds showed that the two chains units of Schiff base exist in the outside of the cavity of pillar[5]arene. Furthermore, the complexing ability of these Schiff bases to transition metal ions were investigated by UV and fluorescence spectroscopy.  相似文献   

11.
Skeletal isomerization of arylsilanes that occurs under conditions of catalytic dehydrocyclization and is accompanied by migration of the triorganosilyl group was additionally confirmed by dehydrocyclization of dimethyl(2,4-dimethylphenyl)(1-naphthyl)silane on chromium-containing oxide catalysts. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2236–2239, December, 1997.  相似文献   

12.
Five metal-bridged biferrocene complexes of the Schiff-base ligand (HL = S-benzyl-N-(ferrocenyl-1-methyl-methylidene)dithiocarbazate) have been studied by single crystal X-ray diffraction and 57Fe Mössbauer spectroscopy. The crystal structures of the complexes show that the central metal ions are tetra-coordinated by two ligands in two modes: the central d8 transition metal ions (Ni2+, Pd2+, and Pt2+) are nearly square-planar coordinated and the d10 transition metal ions (Zn2+ and Cd2+) are tetrahedrally coordinated. Interestingly, the isomer shifts in 57Fe Mössbauer spectroscopy are also of two kinds: d8 transition metal ions (0.097-0.247 mm/s) and d10 transition metal ions (0.416-0.435 mm/s).  相似文献   

13.
本文在研究[PPh4][Cp*MS3](M=Mo,W)配体与铜(银,金,钯)盐及其配合物反应的同时,根据簇合物中所含的金属原子核数,把合成的23个簇合物合成九类(即:MM′型,MM2′型,MM′3型,M2M′3型,M2M′6型,M3M′6型,M3M′7型,M4M′4型,M4M′8型),并对各类簇合物的典型结构特征进行了总结。  相似文献   

14.
Methyl 1,2,3,4-thiatriazol-5-ylcarbamate (2a), ethyl 1,2,3,4-thiatriazol-5-ylcarbamate (2b), 2-butyl 1,2,3,4-thiatriazol-5-ylcarbamate (2c), allyl 1,2,3,4-thiatriazol-5-ylcarbamate (2d), and 3-(1,2,3,4-thiatriazol-5-yl)oxazolidin-2-one (2e) were synthesized with high yields by the reaction of the corresponding carbon(isothiocyanatidic) acid, alkyl esters, and sodium azide in aqueous solution. The compounds were characterized by 1H, 13C, and 15N NMR, vibrational spectroscopy (IR), and single crystal X-ray diffraction. The thermal stability was investigated by differential scanning calorimetry.  相似文献   

15.
Summary Condensation of cyano acid hydrazide1 with cyclopentanone in refluxing ethanolic piperidine yields hydrazone2. With mixtures of aliphatic aldehydes and different active methylene reagents,2 reacts to 1,2,4-triazolo[1,5-a]pyridines (8a–f). Compound2 also reacts with arylidenes9a–g to give triazolopyridines10a–g. Reaction of2 with aromatic aldehydes affords compounds13a–c. Diazotation of2 with aryldiazonium chloride in ethanol at 0 °C leads to the azo adducts15a–d. The thieno-1,2,4-triazolopyridine16 is obtained by reaction of8a with elementary sulfur.16 undergoes cycloaddition with -nitrostyrene, maleic anhydride, N-arylmalemide, and acrylonitrile yielding the isoquinolines21–24. All new compounds have been characterized by their IR,1H NMR, and mass spectra.
Ein neuer Syntheseweg für 1,2,4-Triazolo[1,5-a]pyridine und 1,2,4-Triazolo[1,5-a]isochinoline
Zusammenfassung Kondensation des Cyanohydrazids1 mit Cyclopentanon in ethanolischem Piperidin bei Rückflußtemperatur ergibt das Hydrazon2. Mit Gemischen aus aliphatischen Aldehyden und verschiedenen Verbindungen mit aktiven Methylengruppen reagiert2 zu 1,2,4-Triazolo[1,5-a]pyridinen (8a–f). Verbindung2 reagiert außerdem mit den Arylidenen9a–g zu den Triazolopyridinen10a–g. Umsetzung von2 mit aromatischen Aldehyden führt zu den Verbindungen13a–c. Diazotierung von2 mit Aryldiazoniumchloriden in Ethanol bei 0°C ergibt die Azoaddukte15a–d. Das Thieno-1,2,4-triazolylpyridin16 erhält man durch Reaktion von8a mit elementarem Schwefel.16 geht it -Nitrostyrol, Maleinsäureanhydrid, N-Arylmaleimid und Acrylnitril eine Cycloaddition zu den Isochinolinen21–24 ein. Alle neuen Verbindungen wurden durch ihre IR-,1H-NMR- und Massenspektren charakterisiert.
  相似文献   

16.
An analysis of the structures of minerals with [Hg2]2+ dumbbells including poyarkovite [Hg2]3Cl2O2, shakhovite [Hg2]2Sb(OH)3O3, vasilyevite Hg20O6I3Br2Cl(CO3), and kelyanite [Hg2]6[SbO6]BrCl2 was carried out. The determining factor in structure formation is the ordering of the centers of the cluster groups of mercury and large anions by systems of equidistant parallel planes with d hkl ~ 2.5–4.5 Å. The different combinations of atoms and fragments in the structure are ordered by their own pseudotranslation lattices; this probably reflects the stages of crystallization. The crystal structures under study are examples of balance between the local interatomic interactions and the forces that create long-range order for different stoichiometries, masses, and sizes of components.  相似文献   

17.
The structures of dimers formed from 2,5-di-tert-butylcyclopentadienone in the reaction with alkaline metals and in the Diels-Alder reaction were studied. A photochemical rearrangement with ring contraction was found for the second dimer. Spectral features of the dimers related to steric hindrance were studied by 1D and 2D NMR procedures.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2179–2183, October, 2004.  相似文献   

18.
The first supramolecular adduct (H3O)2[Cu(H2O)4](SO4)2·2(C30H30N20O1024(H2O) based on cucurbit[5]uril was synthesized and characterized by single crystal X‐ray diffraction analysis. In the adduct, copper ion is coordinated by four oxygen atoms from H2O. The latter links two cucurbit[5]uril molecules due to a complicated hydrogen bonding containing lattice water molecules.  相似文献   

19.
Hexane-2,5-dione or 1,1,1,10,10,10-hexafluorodecane-2,4,7,9-tetrone react with methyl trifluoroacetate in the presence of LiH to give, upon treatment with diluted acid, 6-hydroxy-9-oxo-2,4,10-tris(trifluoromethyl)-3,11,12-trioxatetracyclo[5,2,1,02,6,04,10]dodecane. The structure of this compound was determined by X-ray diffraction study.  相似文献   

20.
13C NMR chemical shifts have been measured and assigned for epimeric methyl 3α/β-hydroxy-5β-cholan-24-oates (methyl lithocholate [3α-OH epimer] and methyl iso-lithocholate [3β-OH epimer]). Their molecular dynamics simulations suggest that for both epimers there exists two predominant gas phase conformations, which have been further forwarded for ab initio/HF optimizations and DFT/GIAO based 13C NMR chemical shift calculations. Excellent linear relationships have been observed between experimental and calculated 13C NMR chemical shifts for both epimers. For methyl lithocholate (MeLC), the other minimum energy conformation equates very well with the single crystal X-ray structure (orthorhombic, space group P212121, unit cell ). The crystalline packing of MeLC consists of continuous parallel intermolecular hydrogen bonded [3α-OH?OC24] head-to-tail polymeric chains, which are further cross-linked by many simultaneous weak C(sp3)H?O-type of interactions.  相似文献   

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