Synthesis of 9,10-diacetylenylanthracenes

Syntheses are reported for 9,10-bis(phenylethynyl)anthracene and its derivatives containing identical and different substituants in the phenyl groups by the acetylenic condensation of 9,10-dibromoanthracene. The introduction of a donor substituent into one phenyl group and a withdrawing substituent into the other leads to a significant shift of the fluorescence maximum toward longer wavelengths.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 6, pp. 1441–1443, June, 1990.     

Synthesis and structures of three heterobimetallic compounds based on a new ferrocenyl pyridine ligand

The reactions of 2-PAMF with metal perchlorates [2-PAMF = (2-pyridylmethylamino)carbonylferrocene] yielded three coordination compounds, M(2-PAMF)₂(CH₃CH₂OH)₂(ClO₄)₂ (M = Co 1, Zn 2, and Cu 3), which were characterized by single crystal X-ray diffraction and IR spectroscopy. Compounds 1 and 2 have similar structures with six-coordinate metals in octahedral geometries. The CuII in 3 possesses a severely distorted octahedral geometry due to Jahn–Teller distortion. Adjacent molecules in the three compounds were linked by intermolecular hydrogen bonds to form a 1-D supramolecular chain.     

Synthesis,molecular and crystal structure of new 9,10-substituted deazaflavins

Cyclocondensation of 6-N-(3-hydroxypropyl)aminouracyl with 2-fluoro- or 2,3-dimethoxy-substituted benzaldehydes provided the corresponding 9,10-substituted 5-deazaflavins {pyrimido[4,5-b]quinoline-2,4-(3H,10H)diones}. X-ray diffraction analysis was carried out for 9-methoxy-10-(3-hydroxy-propyl)-substituted 5-deazaflavin derivative.     

Synthesis and anticancer activity of some new heterocyclic compounds based on 1-cyanoacetyl-3,5-dimethylpyrazole

Research on Chemical Intermediates - The starting 3-(3,5-dimethyl-1H-pyrazol-1-yl)-3-oxopropanenitrile (1) reacts with phenyl isothiocyanate and ethyl bromoacetate to give the corresponding...     

Synthesis and nanostructural characterization of new layered compounds based on molybdenum disulfide and organic dyes

Preparation of new MoS₂ layered compounds, in which organic dyes (rhodamine 6G, oxazine 1, and thionine) were used as the guest components, was successfully realized in two reaction systems differing by the nature of molybdenum disulfide. In one system, MoS₂ was used in the form of single-layer dispersion in aqueous media; in the other system, it was taken in the form of nanodispersed powdered material, res-MoS₂, obtained by exfoliation-restacking procedure and suspended in non-aqueous solvent. Structures of prepared compounds are discussed on the basis of their compositions, X-ray diffraction and high-resolution transmission electron microscopy data. The hybrid compounds formed in single-layer dispersions were found to contain the MoS₂ layers, each of which alternate with dye layer, whereas, in the case of res-MoS₂ the same as well as the other sequences of organic and inorganic layers are formed depending on the reaction conditions. The vicinity of different-thickness domains was revealed within the guest layers of rhodamine and oxazine. It results from different packings of organic molecules and sufficient flexibility of molybdenum disulfide layers.     

Synthesis and crystal structure of inclusion compounds: Trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid with boric acid and tetrabutylammonium salt

Two new inclusion compounds (n-C₄H₉)₄N⁺C₁₈-H₁₃O₄ ⁻·B(OH)₃ (1) and (n-C₄H₉)₄N⁺C₁₈H₁₃O₄ ⁻ (2) were prepared and characterized by X-ray crystallography. Crystal data: compound 1, monoclinic P2(1)/c, a = 1.569 9(1) nm, b = 0.995 5(6) nm, c = 2.293 3(1) nm, β = 109.962(3)°, Z = 4, and R ₁ = 0.0434, wR = 0.075 9; compound 2, monoclinic C2/c, a = 1.400 5(3) nm, b = 1,282 1(2) nm, c = 1.765 7(3) nm, β = 100.388(1)°, Z = 4, and R ₁ = 0.0584, wR = 0.096 6. In the crystal structure of 1, the tetramers formed by two trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid (EADA) anions and two boric acid molecules were connected through O—H⋯O hydrogen bonds to generate a channel type host lattice. The tetra-n-butylammonium cations were stacked to give two columns within each channel with cross-sectional size of about 2.30 nm × 0.93 nm. In the crystal structure of 2, similar honeycomb host lattices with big size were also formed along the [101] direction by three-dimensional accumulation of EADA anions. The tetra-n-butylammonium cations were accommodated in a zigzag fashion within each channel. Translated from Acta Chimica Sinica, 2006, 64(18): 1904–1910 [译自: 化学学报]     

Synthesis of 9,10-anthracenedione diethyldithiocarbamates

Russian Journal of General Chemistry -     

Synthesis of new layered-type and new mixed-layered-type bismuth compounds

Four new compounds, PbBi₂TiTaO₈F, PbBi₂TiNbO₈F, Bi₅Ti₂WO₁₄F, and Bi₇Ti₅O₂₀F, were prepared and identified by X-ray diffraction analysis. Two of them are new members of a family called layered bismuth compounds. The other two are new members of a family called mixed-layered bismuth compounds. Thermal properties of the new compounds were studied. Moreover, the possibility of the existence of other new members belonging to the family called mixed-layered bismuth compounds is discussed.     

Synthesis and structure of 9,10-bis(2,4,6-triisopropylphenyl)-9,10-dihydro-9,10-disilaanthracene

We prepared a 9,10-dihydro-9,10-disilaanthracene (DSA) derivative 4 bearing a bulky aryl substituent, a 2,4,6-triisopropylphenyl (Tip) group, on the silicon atoms via a Wurtz-type coupling reaction between two molecules of (2-chlorophenyl)(2,4,6-triisopropylphenyl)silane (3) in a head-to-tail fashion. The structural determination of cis-4 and trans-4 was examined using ¹H NMR spectroscopy and theoretical calculations. In addition, the molecular structure of cis-4 was unambiguously determined by X-ray crystallography. The tricyclic DSA skeleton of cis-4 adopts a folded structure with a boat-like central ring in which the rotation about the Si-Tip bond is restricted. In contrast, theoretical calculations suggest that the tricyclic DSA skeleton of trans-4 has an almost planar structure.     

有机锗硫杂环戊酮化合物的合成

合成了14个1,1-二氯-1,2-锗硫杂-3-环戊酮等四类新型锗硫杂五元环化合物, 元素分析、红外光谱、氢核磁共振谱以及质谱分析验证了它们的组成及结构。     

Phthalocyanines and related compounds: XLI. Synthesis of 9,10-diphenylanthracene-2,3-dicarboxylic acid derivatives

Derivatives of 9,10-diphenylanthracene-2,3-dicarboxylic acid were synthesized by the Diels-Alder reaction of 1,3-diphenylisobenzofuran with adducts of furan (or silvan) and the corresponding maleic (fumaric) acid derivative or with trans-cyclohex-4-ene-1,2-dicarbonitrile, followed by aromatization.     

Synthesis of coumarin based fluorescent compounds

The reaction of different 7,8-disubstituted coumarin 4-acetic acids with 7-diethylaminocoumarin-3-carbaldehyde in the presence of piperidine in methanol gives highly fluorescent (E)-1-(7-diethylaminocoumarin-3-yl)-2-(7,8-disubstituted coumarin-4-yl)ethenes in good yield. Only the (E) diastereomers of these are obtained. The compounds are new, orange to red in colour and show emission in yellow to red region. These compounds were further studied for their emission properties.     

Synthesis and characterization of new cyclotriphosphazene compounds

In the present study, spiro (1a), dispiro (1b, 2, 3), per-substituted spermine-bridged (6–9) and dispiroansa spermine (10) derivatives of cyclotriphosphazene have been synthesized. The structures of the novel compounds (1b, 6–10) have been characterized by elemental analysis, FTIR, mass spectrometry, ¹H and ³¹P NMR spectroscopy. The molecular structures of 1b, 2, 8, and 10 were determined by single crystal X-ray crystallography. In order to investigate the anti-tumour properties of the newly synthesized cyclotriphosphazene derivatives, in vitro cytotoxic activity test (MTT assay) has been performed using HT-29 (human colon adenocarcinoma) and Hep2 (human epidermoid larynx carcinoma) cell lines. The result of the MTT assay showed that while compound 1a has cytotoxic effect on both Hep2 and HT-29 cell lines, compound 3 has only cytotoxic effect towards the Hep 2 cells.     

Synthesis, structure, and catalytic activity of titanium complexes with new chiral 11,12-diamino-9,10-dihydro-9,10-ethanoanthracene-based ligands

A new series of organo-titanium complexes have been prepared from the reaction between Ti(NMe₂)₄ and C₂-symmetric ligands, (R,R)-11,12-bis(pyrrol-2-ylmethyleneamino)-9,10-dihydro-9,10-ethanoanthracene (1H₂), and (R,R)-bis(diphenylthiophosphoramino)-9,10-dihydro-9,10-ethanoanthracene (2H₂), (R,R)-11,12-bis(mesitylenesulphonylamino)-9,10-dihydro-9,10-ethanoanthracene (3H₂) and (R,R)-bis(diphenylthiophosphoramino)-1,2-cyclohexane (4H₂). Treatment of Ti(NMe₂)₄ with 1 equiv of 1H₂ gives, after recrystallization from a benzene solution, the binuclear double helicate titanium amide (1)₂[Ti(NMe₂)₂]₂⋅(5) in 71% yield. While under similar reaction conditions, reaction of Ti(NMe₂)₄ with 1 equiv of 2H₂, 3H₂ or 4H₂ gives, after recrystallization from a toluene or benzene solution, the mononuclear single helicate titanium amides (2)Ti(NMe₂)₂ (6), (3)Ti(NMe₂)₂ (7) and (4)Ti(NMe₂)₂ (8), respectively, in good yields. All new compounds have been characterized by various spectroscopic techniques, and elemental analyses. The solid-state structures of complexes 5-8 have further been confirmed by X-ray diffraction analyses. The titanium amides are active catalysts for the polymerization of rac-lactide, leading to the isotactic-rich polylactides.