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  • 1
    ISSN: 1434-4475
    Keywords: Keywords. Heck reaction; 1-Chloroalk-1-ynes; Cycloalkenes; Cycloalkadienes; Enynes..
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung.  Die Heck-Reaktion zwischen 1-Chlor-2-phenylacetylen und Cycloalkenen oder Cycloalkadienen ergibt phenylethinylsubstituierte Cycloalkene als normale Heck-Produkte sowie 1,3-diphenylprop-2-inyliden- und (cycloalkenyl)phenylmethyliden-substituierte Bicyclen als Tandemprodukte der Reaktion von ClC*CPh und Cycloalkenen im Molverhältnis von 1:2 bzw. 2:1..
    Notes: Summary.  The Heck reaction between 1-chloro-2-phenylacetylene and cycloalkenes or cycloalkadienes affords phenylethynyl substituted cycloalkenes as regular Heck products as well as 1,3-diphenylprop-2-ynylidene and (cycloalkenyl)phenylmethylidene substituted bicyclic compounds as tandem products by reaction of ClC*CPh and the cycloalkene in a ratio of 1:2 and 2:1, respectively..
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  • 2
    ISSN: 0941-1216
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bromination of the disubstituted 4,5-dimethyl-1,3-cyclohexanedione (6) followed by oxidation of the resulting 3-bromo-5,6-dimethyl-2-cyclohexen-1-ones (7) gave 5-bromo-2,3-dimethylphenol (1) together with its constitutional isomer 3. The structure of 1 was secured by a x-ray analysis of its tosyl derivative 8.
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  • 3
    ISSN: 1434-193X
    Keywords: 1,2-Dithiins ; Thiophenes ; Episulfides ; Ring transformation ; Valence isomerization ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Whereas 3,4-bis(p-dimethylaminophenyl)-1,2-dithiete (18) is in equilibrium with its ring-opened valence isomer 19/19′, which can also exist as a solid, the analogously disubstituted 1,2-dithiin 20 is stable when protected from light, but on exposure to light undergoes immediate ring transformation to 2,5-bis(p-dimethylaminophenyl)thiophene-3-thiol (30). To a lesser extent, it also undergoes sulfur extrusion to form 2,5-bis(p-dimethylaminophenyl)thiophene (29). The ring-opened valence isomer 21/21′ and dihydrothiophene episulfide 28 are suggested as key intermediates. X-ray crystallography of the disulfide 31 obtained from the main product 30 unequivocally confirms the structure. The synthesis of 20 is based on the nucleophilic addition of 1,1-dimethylethanethiol to 1,4-bis(p-dimethylaminophenyl)butadiyne (23a) with ensuing functional group conversion. An efficient variant of this method using ethoxycarbonylsulfenyl chloride as a deprotecting reagent is described, leading to the synthesis of 3,6-diphenyl-1,2-dithiin (27).
    Additional Material: 1 Ill.
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  • 4
    ISSN: 1434-1948
    Keywords: Metalla-β-diketones ; Platinum ; Bis(acyl)-bridged complexes ; Platinum blues ; Metal-metal interactions ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The platina-β-diketone [Pt2{(COMe)2H}2(μ-Cl)2] (1) reacts with aliphatic amines [nBuNH2, (iPr)2NH, NEt3], N-methylaniline, and N,N-dimethylaniline, as well as with strong bases, such as a proton sponge or [NMe4]OH, in an equimolar ratio to give the anionic platina-β-diketonato complexes of platina-β-diketones [BH]2[{Cl2Pt(μ-COMe)2Pt[(COMe)2H]}2] (3) {B = nBuNH2 (3a), (iPr)2NH (3b), NEt3 (3c), PhNHMe (3d), PhNMe2 (3e), C10H6(NMe2)2 [1,8-bis(dimethylamino)naphthalene] (3f) and [NMe4]2[{Cl2Pt(μ-COMe)2Pt[(COMe)2H]}2] (3g)}. All complexes were characterized by microanalysis, and by 1H-NMR and IR spectroscopy. X-ray structure analyses reveal that in the solid state the complexes 3a · 0.5 CH2Cl2 and 3g · 2 CH2Cl2 consist of tetranuclear dianions with zigzag Pt4 chains [Pt-Pt-Pt angle: 122.92(3)° (3a), 119.30(6)° (3g)]. The central Pt···Pt distances [3a: 3.171(1) Å, 3g: 3.176(1) Å] give evidence for closed shell d8-d8 interactions. Thus, these bis(acyl)-bridged complexes can be regarded as organometallic analogues of platinum blue complexes.
    Additional Material: 2 Ill.
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  • 5
    ISSN: 0044-8249
    Keywords: Bioanorganische Chemie ; Kohlenhydrate ; O-Liganden ; Platin ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 6
    ISSN: 1572-901X
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract [K(18-cr-6)]2[Pt2Cl6] reacts with olefins in CH2Cl2 to give crown ether adducts of olefin complexes of Zeise's salt type [K(18-cr- 6)][PtCl3(olefin)] (2) [olefin: EtCH=CH2 (2a), cis-MeCH=CHMe (2b), trans-MeCH=CHMe (2c), nPrCH=CH2 (2d), cis-EtCH=CHMe (2e), trans-EtCH=CHMe (2f), nBuCH=CH2 (2g), cis-nPrCH=CH-Me (2h), cis-EtCH=CHEt (2i), trans-EtCH=CHEt (2j), cyclohexene (2k), PhCH=CH2 (2l)]. The complexes were characterized by microanalysis, n.m.r. (1H, 13C) and i.r. spectroscopy. The crystal structures of the cis-but-2-ene (2b) and cis-pent-2-ene complexes (2e) were determined by single-crystal X-ray analyses. The Pt atom is square-planar, coordinated by three chloro ligands and the olefin ligand [interplanar angle PtCl3/Pt(C=C) 89.6° (2b), 86.6° (2e)]. The C=C bond length is 1.38(1)Å (2b) and 1.32(2)Å (2e), respectively. The substituents (Me, Et) on the double bond are bent back away from Pt [torsion angles C–C=C–Pt 109(2)–110.7(8)°]. There are close contacts of the [K(18- cr-6)]+ cations both to the trans and one of the cis chloro ligands [K···Cl 3.208(2)/3.230(2)Å (2b); 3.220(5)/3.370(5)Å (2e)].
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  • 7
    ISSN: 0570-0833
    Keywords: bioinorganic chemistry ; carbohydrates ; O ligands ; platinum ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 8
    ISSN: 0044-2313
    Keywords: Aquapentachloroplatinates(IV) ; (18-crown-6)-potassium-aquapentachloroplatinate ; crown ether complexes ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Characterization of Aquapentachloroplatinates(IV) - Structure of [K(18-crown-6)][PtCl5(H2O)]The crown ether complex of the aquapentachloroplatinic acid of the composition [H13O6][PtCl5(H4O2)] · 2(18-cr-6) (2) reacts with K2CO3 and [NnBu4]OH in aqueous solution to give [K(18-cr-6)][PtCl5(H2O)] (5 a) and [NnBu4][PtCl5(H2O)] · 1/2 (18-cr-6) · H2O (5 b), respectively. Both compounds were characterized by microanalysis, vibrational (IR, Raman) and NMR (1H, 13C, 195Pt) spectroscopy. The X-ray structure analysis of 5 a (orthorhombic, pnma; a = 16,550(4), b = 18,044(3), c = 7,415(1) Å; Z = 4; R1 = 0,0183; wR2 = 0,0414) reveals that the crystal is threaded by chains built up of [PtCl5(H2O)]- and [K(18-cr-6)]+ units. There are tight K … Cl contacts (d(K—Cl1)) = 3,0881(9) Å and OW—H—Ocr hydrogen bridges (d(O1 … O2) = 2,806(3) Å) between these units. The coordination polyhedron [PtCl5O] has approximately C4v symmetry.
    Notes: Der Kronenetherkomplex der Aquapentachloroplatinsäure mit der Zusammensetzung [H13O6][PtCl5(H4O2)] · 2(18-cr-6)Abkürzungen: 18-cr-6 = 18-Krone-6; OW, Ocr = Sauerstoff von Wasser bzw. Kronenether. (2) reagiert mit K2CO3 und [NnBu4]OH in wäßriger Lösung zu [K(18-cr-6)][PtCl5(H2O)] (5 a) bzw. zu [NnBu4][PtCl5(H2O)] · 1/2 (18-cr-6) · H2O (5 b). Beide Verbindungen wurden durch Elementaranalyse sowie schwingungs- (IR, Raman) und NMR-spektroskopisch (1H, 13C, 195Pt) charakterisiert. Die Röntgenkristallstrukturanalyse von 5 a (orthorhombisch, Pnma; a = 16,550(4), b = 18,044(3), c = 7,415(1) Å; Z = 4; R1 = 0,0183; wR2 = 0,0414) zeigt, daß der Kristall von Ketten durchzogen wird, die aus [PtCl5(H2O)]- und [K(18-cr-6)]+ Einheiten aufgebaut sind. Zwischen ihnen bestehen enge K … Cl Kontakte (d(K—Cl1) = 3,0881(9) Å) sowie OW—H—Ocr Wasserstoffbrücken (d(O1 … O2) = 2,806(3) Å). Für das koordinationspolyeder [PtCl5O] kann näherungsweise C4v-Symmetrie angenommen werden.
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  • 9
    ISSN: 0044-2313
    Keywords: Phthalocyaninates(2-) ; ruthenium compounds ; iron compounds ; vibrational spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Properties, and Crystal Structure μ-Carbidodi(pyridinephthalocyaninato(2-)iron(IV)) and -ruthenium(IV))Soluble μ-carbidodi(pyridinephthalocyaninato-(2-)iron(IV)) and -ruthenium(IV) is prepared as a pyridine solvate, [{M(py)pc2-)2(μ-C)] · py (M = Fe, Ru) by the reaction of μ-carbidodi(phthalocyaninato(2-)iron(IV)) and -ruthenium(IV)) with pyridine. The isotypic complexes crystallize in the orthorhombic space group P212121 (No. 19) with lattice parameters (in Å): a = 12.692(3)713.002(3) (Fe/Ru); b = 22.186(2)722.635(6); c = 23,653(2)/23.901(6). The M atoms are virtually in the centre (Ct) of the (Np)4 plane (d(M-Ct) = 0.039(6)70.054(8) Å; Np: pyrrole-N atom). The averaged (M-Npy) distance (py: pyridine) is 1.94(1)/2.010(8) Å. The M-(μ-C)-M core is almost linear. The (M-(μ-C)) distance is 1.69(2)71.77(1) Å. The pc2- ligands are in a hitherto unknown convex staggered conformation. The asymmetric (M-(μ-C)-M) stretching vibration is observed in the IR spectrum at 9117974 cm-1, while the corresponding symmetric one is selectively enhanced only in the RR spectrum at 477 cm-1 of the iron complex.
    Notes: Lösliches μ-Carbidodi(pyridinphthalocyaninato(2-)eisen(IV) und -ruthenium(IV) wird durch die Umsetzung von μ-Carbidodi(phthalocyaninato(2-)eisen(IV) und -ruthenium(IV) mit Pyridin als Pyridin-Solvat, [{M(py)pc2-}2(μ-C)] · py (M = Fe, Ru) isoliert. Die isotypen isotypen Komplexe kristallisieren orthorombisch in der Raumgruppe P212121 (Nr. 19) mit den Gitterkonstanten (in Å): a = 12,692(3)/13,002(3) (Fe/Ru); b = 22,186(2)/22,635(6); c = 23,653(2)/23,901(6). Die M-Atom befinden sich fast im Zentrum (Ct) der (Np)4-Ebene (Np: Pyrrol-N-Atom): d(M-Ct) = 0,039(6)/0,054(8) Å. Der mittlere (M-Np)-Abstand beträgt 1,94(1)/2,010(8) Å. Die (M-(μ-C)-Abstand beträgt 1,69(2)/1,77(1) Å. Die pc2--Liganden sind in einer bislang unbekannten komplexen Staffel-Konformation einander zugeneigt. Die asymmetrische (M-(μ-C)-M)-Valenzschwingung liegt im IR-Spektrum bei 911/974 cm-1, die symmetrische beobachtet man dagegen nur im RR-Spektrum des Eisen-Komplexes bei 477 cm-1.
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  • 10
    ISSN: 1573-8353
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Reaction of [PtMe3(Me2CO)3]BF4 (1) with 3-O-acetyl-1,2;5,6-di-O-isopropylidene-α-D-glucofuranose in acetone affords [PtMe3L]BF4 (2) (L=3-O-acetyl-1,2-O-isopropylidene-α-D-glucofuranose). In wet methylene chloride, complex2 transforms to [PtMe3L(H2O)]BF4·H2O (3). Complex3 was characterized by microanalysis and NMR spectroscopy (1H,13C,195Pt). The X-ray structure analysis (monoclinic, P21, a=10.529(3) Å, b=7.322(2) Å, c=14.668(4) Å, Z=2) reveals that 3-O-acetyl-1,2-O-isopropylidene-α-D-glucofuranose acts as a neutral bidentate ligand which is coordinated via two hydroxyl groups (κ2O5,6 coordination). The five-membered 1,3,2-dioxaplatina rings exhibit an envelope conformation. The coordination sphere of platinum is completed by H2O ligand.
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