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1999 (254)
61Author    Z. NaturforschRequires cookie*
 Title    Untersuchungen zur Trifluoracetylierung der Methylderivate von Tryptamin und Serotonin mit verschiedenen Derivatisierungsreagentien: Synthesen, Spektroskopie sowie analytische Trennungen mittels Kapillar-GC  
 Abstract    Die Trifluoracetylierungs-Reaktionen verschiedener N-Methylderivate des Tryptamins so­ wie von N-und O-Methylderivaten des Serotonins mit den Derivatisierungsreagentien: Tri-fluoracetanhydrid, N-Methylbistrifluoracetamid und Trifluoracetylimidazol wurde analytisch mittels Glas-Kapillar-GC untersucht und die Strukturen der trifluoracetylierten Reaktions­ produkte durch GC-MS-Kombination ermittelt. Fünf dieser Trifluoracetylderivate wurden außerdem präparativ dargestellt und durch MS, IR, 1H, 13C und 19F NMR-Spektren charakte­ risiert. Im Gegensatz zu Literaturangaben lassen sich die physiologisch interessanten Indol-ethylamine mit einer tertiärer Dimethylaminoseitenkette (z.B. DMT und Bufotenin) nicht unter den gleichen Reaktionsbedingungen wie bei den anderen Methylderivaten trifluorace-tylieren, da die tertiäre Aminogruppierung eine Trifluoracetylierungsreaktion eingeht. Das entsprechende nichtflüchtige N-trifluoracetylierte Produkt wurde von uns präparativ isoliert und spektroskopisch eindeutig charakterisiert. 
  Reference    Z. Naturforsch. 54b, 397—414 (1999); eingegangen am 13. November 1998 
  Published    1999 
  Keywords    Analytical and Preparative Trifluoroacetylation, Trifluoroacetic Anhydride, N-Methylbistri-fluoroacetamide, Trifluoroacetylimidazole, Methylated Tryptamines 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0397.pdf 
 Identifier    ZNB-1999-54b-0397 
 Volume    54 
62Author    Z. Afar Iqbalc, H.E JRequires cookie*
 Title    Isoperadione: A New Triterpenoid from Salvia bucharica  
 Abstract    V iqar U d d in A h m a d 3 *, M uham m ad Z ah id c, M uham m ad Shaiq A li3, Z ulfiqar A li3, N aseer A lam 3, R asool B akhsh T areenb, M uham m ad A new isomer of peradione (2) named as isoperadione (1) has been isolated along with peradione (2) and perovskone (3) from the hexane soluble part of Salvia bucharica. The structures of 1 -3 were elucidated with the aid of modern spectroscopic techniques. 
  Reference    Z. Naturforsch. 54b, 415—418 (1999); received September 8 1998 
  Published    1999 
  Keywords    Salvia bucharica, Lamiaceae, Triterpenoids, Isoperadione, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0415.pdf 
 Identifier    ZNB-1999-54b-0415 
 Volume    54 
63Author    Z. NaturforschRequires cookie*
 Title    Synthese von muscarinanalogen Epoxiden aus Campholen- und Fencholenverbindungen  
 Abstract    Synthesis of M uscarin A nalogue Epoxides from C am pholenic and Fencholenic C om pounds K atrin A n h a lt3, K laus Schulze3, P eter Jörchel5, M arijana G avranic3 Muscarin, Cyclopentene Epoxide, Trimethylammonium Iodide, Campholenic and Fencholenic Derivatives In connection with the synthesis and epoxidation of campholenic and fencholenic derivati­ ves some trimethylammonium iodides (2 and 4) similar to muscarin were prepared. They may be of interest for the investigation of the cholinergic receptor. The stereochemistry of the epoxytrimethylammonium iodide 4a was determined by NMR and X-ray analysis. 
  Reference    Z. Naturforsch. 54b, 419—423 (1999); eingegangen am 13. Oktober 1998 
  Published    1999 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0419.pdf 
 Identifier    ZNB-1999-54b-0419 
 Volume    54 
64Author    2. 2., Z. NaturforschRequires cookie*
 Title      
 Abstract    -/erf-butyI-3,3'-bis(tri-m e th y lsily l)-l,l'-diazacobaltocen [1 ] 2.2..5.5'-Tetra-terr-butyl-3,3,-bis(tri-m eth y lsily l)-l,r-d iazaco b alto cen e [1] N o rb ert K uhn3 *, Stefan S tubenrauchb, D ieter B läserc, R oland B oesec The 1,1'diazacobaltocene pyr2Co (3) is obtai­ ned from the reaction of 2,5-di-terr-butyl-3-trime-thylsilylpyrrole (pyrH, 2) and CoCl2. The X-ray structure is reported. 
  Reference    Z. Naturforsch. 54b, 424—426 (1999); eingegangen am 5. November 1998 
  Published    1999 
  Keywords    Heterocycles, Pyrroles, Cobalt X-Ray Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0424_n.pdf 
 Identifier    ZNB-1999-54b-0424_n 
 Volume    54 
65Author    N. Orbert, K. Uhn, M. Anfred, Steim Ann, Gerd Weyers, HerrnRequires cookie*
 Title    Synthese und Eigenschaften von l,3-Diisopropyl-4,5-dimethylimidazolium- 2-car boxy lat. Ein stabiles Carben-Addukt des Kohlendioxids [1]  
 Abstract    The reaction of 2,3-dihydro-l,3-diisopropyl-4,5-dimethylimidazol-2-ylidene (5) with C 0 2 gives the imidazolium-2-carboxylate 6 . The compound can be transformed into the salts of its corresponding Broenstedt acid 8 . The cationic acid chloride 10a is obtained from 6 and thionyl chloride. Chemical properties and spectroscopic data indicate 6 to be less basic than its anionic counterparts, e. g. PhC02 . The X-ray structure of 
  Reference    Z. Naturforsch. 54b, 427—433 (1999); eingegangen am 27. November 1998 
  Published    1999 
  Keywords    Carbenes, Imidazoles, Carboxylic Acids, X-Ray Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0427.pdf 
 Identifier    ZNB-1999-54b-0427 
 Volume    54 
66Author    Norbert Kuhn, Manfred Steimann3, Gerd Weyers3, Gerald Henkelh, HerrnRequires cookie*
 Title    l,3-DHSopropyl-4,5-dimethylimidazolium-2-N,N'-diisopropylamidinat, ein neuartiges Retain [1] 1,3-Diisopropyl-4,5-dimethylimidazolium-2-N,N'-diisopropylamidinate, a Novel Betaine [1]  
 Abstract    The imidazolium-2-amidinate 6 is obtained from the reaction of 2,3-dihydro-1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene (4) with diisopropylcarbodiimide (5) as stable solid. Overcrow­ ding causes a lowered symmetry of the amidinate fragment indicated both by structural and NMR data. The strongly basic properties of 6 allow facile protonation with HC1 to the cationic amidine derivatives 7 and 8 . The ketoamidine 10 is formed by a ring opening reaction of 6 with water. I he X-ray structures of 6 and 10 are reported 
  Reference    Z. Naturforsch. 54b, 434—440 (1999); eingegangen am 21. Dezember 1998 
  Published    1999 
  Keywords    Amidines, Carbenes, Carbon Diimides, Imidazoles, X-Ray Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0434.pdf 
 Identifier    ZNB-1999-54b-0434 
 Volume    54 
67Author    KurtO. Klepp, Andreas KolbRequires cookie*
 Title    Komplexe Chalkogenide der IVa Metalle mit niedrigdimensionalen anionischen Partialstrukturen. Darstellung und Kristallstruktur von K2ZrTe3 und Rb2ZrTe3 Complex Chalcogenides of the IVa Metals with Low Dimensional Anionic Partial Structures. Preparation and Crystal Structures of K2ZrTe3 and Rb2ZrTe3  
 Abstract    The isostructural compounds K2ZrTe3 and Rb2ZrTe3 were obtained at 1000°C by reacting K7Te and Rb9Te with stoichiometric amounts of Zr and Te. The compounds are monoclinic, mP24, space group P2,/c, Z = 4 with a = 9.089(3), b = 14.148(4), c = 6.986(3)Ä, ß = 105.90(1)° and a = 9.735(4), b = 14.300(7), c = 6.952(8) Ä, ß = 108.61(2)°, respectively. The crystal structure was determined from diffractometer data and refined to R = 0.030 for 1452 Fo's for K2ZrTe3 and R = 0.038 for 1131 Fo's for Rb2ZrTe3. The crystal structure is of a new type, characterized by infinite anionic chains, ^-[ZrTe3]2_ built up by octahedra sharing opposite faces which run along [001]. The mean Zr-Te bond lengths are 2.921 and 2.920 A, respectively. The alkali cations separating the chains are characterized by two different -distorted octahedral and pentagonal bipyramidal -chalcogen environments. E inleitung 
  Reference    Z. Naturforsch. 54b, 441 (1999); eingegangen am 9. November 1998 
  Published    1999 
  Keywords    Crystal Structure, Complex Chalcogenides, Tellurides, Zirconium, Pseudo-one-dimensional solids 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0441.pdf 
 Identifier    ZNB-1999-54b-0441 
 Volume    54 
68Author    K. O. Kleppa, J. Hieblb, H. Kollmannb, F. RovenszkybRequires cookie*
 Title    The Crystal Structure of Dimethyl (2Z, 6Z)-2,7-bis-(benzyloxycarbonyl- amino)octa-2,6-diendioate: A Useful Precursor for Optically Pure 2,7-Diaminosuberic Acid  
 Abstract    Crystal Structure, Dimethyl (2Z, 6Z)-2,7-bis-(benzyloxycarbonylamino)octa-2,6-diendioate Needle shaped single crystals of the dimethyl ester of (2Z, 6Z)-2,7-bis-(benzyloxycarbonyl-amino)-octa-2,6-diendioic acid (1), C26H28N2O8 were obtained by very slow cooling from methanol/ethylacetate solution 20:1. 1 crystallizes in the anorthic space group Pi (No.2) with a = 4.813(5), b = 12.277(6), c = 12.340(7) A, a =117.15(3)°, f3 = 97.52(4)°, 7 = 92.02(4)°, Z =1. The crystal structure was determined from diffractometer data (MoKa-radiation). It was solved by direct methods and refined to a conventional R of 0.054 for 1452 Fo's and 178 refined parameters. The molecule is characterized by the presence of an inversion center. In the crystal structure the molecules are stacked along the crystallographic a-axis. In this direction -which coincides with the needle axis of the crystals -each molecule is connected with its neighbors through almost linear N-H- • O-hydrogen bonds. 
  Reference    Z. Naturforsch. 54b, 447—450 (1999); received November 12 1998 
  Published    1999 
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 Identifier    ZNB-1999-54b-0447 
 Volume    54 
69Author    VictorA. Trusha, KonstantinV. Domasevitcha, VladimirM. Amirkhanov2, Joachim SielerbRequires cookie*
 Title    Structure of Tl(18-cr0wn-6){Cl3C C (0)N P (0)(0C H 3)2}: Coordination of the Ionic Multidentate Weakens the Interaction of the Metal Atom with the Crown Ether  
 Abstract    The thallium(I) dimethyl-N-trichloroacetylamidophosphate complex with a 18-crown-6 of the composition Tl(18-crown-6){L} (L = {Cl3CC(0)NP(0)(0 CH3)2}_) has been prepared and characterized by means of IR spectroscopy and X-ray diffraction (orthorhombic, space group P2,2,2, with a = 8.660(1), b = 11.557(2), c =26.296(3) A, Z = 4, V = 2631.8(6) Ä3; R\ = 0.0285 and wR2 = 0.0558 for 4314 unique reflections). It was shown that (L~) is coordinatedoto the central atom in a bidentate manner via oxygen atoms of phosphoryl [Tl-O(l) 2.678(4) A] and carbonyl groups [Tl-0(2) 3.012(6) A], The Tl(18-crown-6)+ moiety adopts a typical "sunrise" coordination with the metal atom laying 1.134(2) A above the mean plane of the oxygen atoms of the macrocycle. This deviation is the highest value of the structurally examined Tl(18-crown-6)+ complexes. The Tl-O (etheric) separations are in the range 2.913(4) -3.198(5) A (av. 3.030(6) A). 
  Reference    Z. Naturforsch. 54b, 451—455 (1999); received September 29 1998 
  Published    1999 
  Keywords    Thallium(I), Crown Ethers, Carbacylamidophosphates, X-Ray Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0451.pdf 
 Identifier    ZNB-1999-54b-0451 
 Volume    54 
70Author    IgorO. Fritsky, Aldona Karaczynb, Henryk Kozłowski, Tadeusz Głowiakb, ElenaV. Prisyazhnaya3Requires cookie*
 Title    Crystal and Molecular Structure of Two Tetradentate "Oxime-and-Amide" Ligands  
 Abstract    Tetradentate Ligands, X-Ray Data Syntheses and X-ray structure analyses of two new tetradentate ligands with "oxime-and-amide" donor systems (N,N'-bis(2-hydroiminopropionyl)-l,2-diaminoethane and N,N'-bis(2-hydroxyiminopropionyl)-l,4-diaminobutane) were performed. The overall conformation of both ligands is distinctly different from that reported earlier for N,N'-bis(2-hydroxyimino-propionyl)-l,2-diaminopropane. The number of methylene groups critically influences the lig­ and geometry and may have distinct impact on the co-ordinating ability of the ligands. 
  Reference    Z. Naturforsch. 54b, 456—460 (1999); received November 25 1998 
  Published    1999 
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 Identifier    ZNB-1999-54b-0456 
 Volume    54 
71Author    M. Ludwig3, R. Niewab, R. KniepRequires cookie*
 Title    Dimers [A12N6]12-and Chains J j A lN ^ ] in the Crystal Structures of Ca6[Al2N6] and Ba3[Al2N4]  
 Abstract    Pale yellow transparent single crystals of Ca6[Al2Nö] (P 2\/c, No. 14, a = 693.7(3), b = 614.9(3), c = 987.1(5) pm, ß = 94.01(5)°; Z = 4) and colourless transparent single crystals of Ba.^ALN*] (Pnna, No. 52, a = 617.9(2), b = 1005.2(4), c = 1023.0(4) pm; Z = 4) were obtained from reactions of mixtures of the representative metals with nitrogen at Tmax = 1000 °C. The crystal structure of CaöfALNft] contains isolated units [ALNftJ12-built of two edge-sharing tetrahedra. Ba3[ALN4] is an isotype of S r^A bN ^. The crystal structure contains infinite chains ^ [A1N^T2] of trans edge-sharing tetrahedra. 
  Reference    Z. Naturforsch. 54b, 461—465 (1999); received December 18 1998 
  Published    1999 
  Keywords    Nitridoaluminates, Preparation, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0461.pdf 
 Identifier    ZNB-1999-54b-0461 
 Volume    54 
72Author    IgorL. Fedushkina, MarcWeydertb Anatoly, A. Fagina, SergeiE N Efedovc, IgorL. Eremenko0, MikhailN. Bochkarev3 ', Herbert Schumannb, G. A. RazuvaevRequires cookie*
 Title    Metallation of Calix[4]arene with Thulium Diiodide, TmI2(DME)3 : Molecular Structure of [(5,ll,17,23-Tetra-te/*-butyl-25,27-dioxo-26,28- dimethoxycalix[4]arene)thulium(III)iodide(diethyl etherate)]  
 Abstract    Thulium Diiodide, Calix Arene [(5,11,17,23-Tetra-/e/t-butyl-25,27-dioxo-26,28-dimethoxycalix[4]arene)thulium(III)-iodi-de(diethyl etherate)] 1 is obtained by deprotonation of 5,1 l,17,23-tetra-/m-butyl-25,27-dihydroxy-26,28-dimethoxy-calix[4]arene with 2 equivalents of Tml2(DME)3 in THF. 
  Reference    Z. Naturforsch. 54b, 466—468 (1999); received December 23 1998 
  Published    1999 
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 Identifier    ZNB-1999-54b-0466 
 Volume    54 
73Author    B. Wedelb, K. Sugiyama3, K. Hiraga3, K. ItagakibRequires cookie*
 Title    Zur Kristallchemie des ersten Blei-Zink-Silicium-Telluroxids: PbZn4SiTeOio On the Crystal Chemistry o f the First Lead Zinc Silicon Tellurium Oxyde PbZn4SiTeO 10  
 Abstract    Single crystals of the new lead zinc silicon tellurium oxide PbZn4SiTeO10 have been prepared by solid state reaction in air. The compound is colourless and crystallizes in orthorhombic symmetryj space group Dih Pnma, with the cell parameters: a = 6.542 (5), b = 15.624(4), c = 8.280(4) A, Z = 4. The structure has been determined from a single crystal X-ray study and refined to the conventional values R = 0.032 and wR(F2) = 0.050. Zn~+ and Si4+ show tetrahedral and Te6+ octahedral coordination by 0 2~.The crystal structure is dominated by a ^ [Zn4O l0]12-framework with isolated Te066+ and Si044+ polyhedra. Pb2+ ions are incorporated in the network. The centres of negative charge of the lone of the Coulomb term of the lattice energy. 
  Reference    Z. Naturforsch. 54b, 469—472 (1999); eingegangen am 3. Dezember 1998 
  Published    1999 
  Keywords    Lead, Zinc, Silicon, Tellurium, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0469.pdf 
 Identifier    ZNB-1999-54b-0469 
 Volume    54 
74Author    Cornelia Borgmann, Christian Limberg, Läszlö Zsolnai, Katja HeinzeRequires cookie*
 Title    Syntheses, Structures, and Spectroscopic Properties of Alkoxide, Hydroxide, and Siloxide Complexes with (r73-Allyl)Mo Moieties  
 Abstract    Salts with binuclear anions of the general formula [(?73-C3H4R)(CO)2Mo(^-OR')2(/i-OR")-Mo(CO)2(f?3-C3H4R) r (R = h , R',R" = Me, 2 ; R = CH3, R' = CH(CH3)2, R" = OH, 3; R = CH3, R' = OH, R" = OSiMe3, 4) have been synthesised via reaction of [(r/3-C3H4R)-Mo(CO)2(CH3CN)2(thf)]+BF4_ , 1, with NaOMe, NaO'Pr, and KOSiMe3. All products were characterised spectroscopically and investigated by single crystal X-ray analysis. In the case of 3 low temperature 2D-NMR spectra revealed that the solid state structure is maintained in solution and that the compound shows a trigonal twist-rearrangement at room temperature. 
  Reference    Z. Naturforsch. 54b, 473—481 (1999); received October 28 1998 
  Published    1999 
  Keywords    Molybdenum Complexes, Allyl, Alkoxides, Hydroxides, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0473.pdf 
 Identifier    ZNB-1999-54b-0473 
 Volume    54 
75Author    Markus Häp, TheoG. Illes, Thomas Kruck, Karl-Friedrich TebbeRequires cookie*
 Title    Dichloro  
 Abstract    [bis(775-2,4-cyclopentadien-l-yl)aIkylphosphan]zirconium: PR(C5H4)2 ZrCl2 ; R = Me, Et, 'Pr, 'Bu Dichloro[bis(/7r'-2 ,4 -cyclopentadien-l-yl)alkylphosphine]zirconium: PR(C5H4)7ZrCL; R = Me, Et, 'Pr, ?Bu A series of new ansa-zirconocene dichloride compounds [PR(C5H4)2ZrCl2: R = Me (5), Et (6), 'Pr (7), ?Bu (8)] with phosphorus as bridging atom between the cyclopentadienyl rings have been prepared, isolated, and characterised by 'H, i3C, 31P NMR spectroscopy, mass spectrometry and elemental analysis. The X-ray structure of 5 is reported. 
  Reference    Z. Naturforsch. 54b, 482—486 (1999); eingegangen am 22. Dezember 1998 
  Published    1999 
  Keywords    Zirconium Ansa-Metallocene, Cyclopentadienyl, Phosphine, Crystal Structure 
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 Identifier    ZNB-1999-54b-0482 
 Volume    54 
76Author    U. Petasch, H. OppermannRequires cookie*
 Title    Untersuchungen zum quasibinären System Bi2Te3/BiBr3 Investigations on the Pseudobinary System Bi-,Te3/BiBr3  
 Abstract    The phase diagram of the pseudobinary sytem Bi2Te3/BiBr3 was investigated by DTA, total pressure measurements and X-ray phase analysis. Only BiTeBr exists as a ternary phase in this system. The compound melts congruently at 526 °C. The heat of formation and standard entropy were calculated from vapor pressure data: Z\H(BiTeBr, f, 298) = (-30,4 ± 1,4) kcal/mol; S°(BiTeBr, f, 298) = (36,2±2,9) cal/K mol. 
  Reference    Z. Naturforsch. 54b, 487—190 (1999); eingegangen am 15. Januar 1999 
  Published    1999 
  Keywords    Bismuth Telluride Bromide, Phase Diagram, Barogram, Total Pressure Measurements, Thermodynamic Data 
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 Identifier    ZNB-1999-54b-0487 
 Volume    54 
77Author    Hans Bock, Norbert Nagel, Peter Eller, Herrn Professor, Manfred EigenRequires cookie*
 Title    Wechselwirkungen in Molekülkristallen, 153 [1 -3]. Wirt/Gast-Einschlußverbindungen von N,Nf-Ditosyl-/?-phenylendiamin- Derivaten: Die Kristallstrukturen von N,N'-Di(4-ethyl-benzosulfuryl)-/?- phenylendiamin und seinen Aggregaten mit Aceton und Cyclopentanon Interactions in Molecular Crystals, 153 [1 -3]. Host/Guest-Inclusion Compounds of N,N'-Ditosyl-/?-phenylenediamine Derivatives: The Crystal Structures o f N,N'-Di(4-ethyl- benzosulfuryl)-/?-phenylenediamine and its Aggregates with Acetone and Cyclopentanone  
  Reference    Z. Naturforsch. 54b, 491—500 (1999); eingegangen am 26. Oktober 1998 
  Published    1999 
  Keywords    N, N'-Di(4-ethyl-benzosulfuryl)-p-phenylenediamine, Inclusion Compounds, Ketone Guest Molecules, Crystal Growth, Structures 
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 Identifier    ZNB-1999-54b-0491 
 Volume    54 
78Author    Hans Bock, Norbert Nagel, Peter Eller, Herrn Professor, Manfred EigenRequires cookie*
 Title    Wechselwirkungen in Molekülkristallen, 154 [1 -3]. Wirt/Gast-Einschlußverbindungen von NjN'-Ditosyl-p-phenylendiamin- Derivaten: Die Kristallstrukturen von N,N'-Di(4-nitro-benzosulfuryl)-/?- phenylendiamin und seinen Wasserstoffbrücken-Addukten mit Cyclo- pentanon, Cyclohexanon, Tetrahydrofuran, N,N-Dimethylformamid- sowie Pyridin Interactions in M olecular Crystals, 154 [1 -3]. Host/Guest-Inclusion Compounds o f N,N'-Ditosyl-/?-phenylenediamine Derivatives: The Crystal Structures o f N,N'-Di(4- nitro-benzosulfuryl)-/?-phenylenediamine and its Hydrogen-Bonded Adducts with Cyclopentanone, Cyclohexanone, Tetrahydrofurane, N,N-Dimethylformamide as well as Pyridine  
  Reference    Z. Naturforsch. 54b, 501—514 (1999); eingegangen am 26. Oktober 1998 
  Published    1999 
  Keywords    N, N'-Di(4-nitro-benzosulfuryl)-p-phenylenediamine, Inclusion Compounds, Hydrogen Acceptor Guest Molecules, Crystal Growth, Structures 
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 Identifier    ZNB-1999-54b-0501 
 Volume    54 
79Author    F. K. Ubela, H. Billb, H. H. Ag, Em AnRequires cookie*
 Title    Low Temperature Crystal Growth and Structure of Ordered Ba7F12Cl2  
 Abstract    of composition Ba7F12Cl2 were obtained by a reaction at room temperature be­ tween Ba2+/Cl"/F_ in a gel of agar-agar/water. The hexagonal crystals have space group P6, «=1064.69(8), c=417.89(5)pm, V=410.24(8) 106 pm3 and Z=l. The anions form a propeller type network located in tunnels parallel to the chex axis; the chloride ions are located at the center on the propeller axes. The Ba2+ ions are coordinated by a (distorted) tricapped trigo­ nal environment of fluoride and chloride anions. Disorder is present for one particular Ba2+ site. The average structure is isotypic with the structure of Pb7F)2Cl2. 
  Reference    Z. Naturforsch. 54b, 515—518 (1999); received November 30 1998 
  Published    1999 
  Keywords    Bariumfluorochloride, Hexagonal Crystal Structure, Crystal Growth, Low Temperature Gel Method Crystals 
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 Identifier    ZNB-1999-54b-0515 
 Volume    54 
80Author    Z. NaturforschRequires cookie*
 Title    Darstellung chiraler heterocyclischer /?-Aminosäureester  
 Abstract    /3-Amino-acid Esters, Bicyclic Heterocyclic Compounds, Intramolecular 1.3-Dipolar Cycloaddition, Nitrones, Stereocontrol Chiral /3-amino alcohols were successively prone to N-benzylation, O-allylation and oxida­ tion of the resulting benzylamino group to give nitrones 3 which on hydrolysis afforded chiral hydroxylamines H0-NH-CH(R)-CH?-0-C H 2-CH=CH2 ((S)-4: R = Me, Bn, /Pr. (R)-4: R = Et). Swern oxidation of methyl 2,2-dimethyl-3-hydroxypropionate (16) and treatment of the resulting aldehyde 17 with hydroxylamines (S)-4b (R = Bn) or (R)-4d (R = Et) provided nitrones 18 that underwent an intramolecular 1,3-dipolar cycloaddition on heating yielding the bicyclic /3-amino-acid esters 19b and ent-19d, respectively. Reductive cleavage of the N,0-bond of compounds 19 afforded the eight-membered ring compounds 20b and ent-20d, re­ spectively. N-Benzylalaninol (22) was treated with /3-bromo-methacrylate to give the amino alcohol 23. Swern oxidation and subsequent treatment with N-ferf-butylhydroxylamine provided the bicyclic ester 26a (R = r-Bu) via the corresponding nitrone 24. Oxime 25 was prepared in an analogous way as 24 with unsubstituted hydroxylamine. It underwent an intramolecular 1.3-dipolar cycloaddition yielding 26b on heating in toluene. Reduction of 26a afforded the pyr-rolidine-carboxylic ester 27a. 
  Reference    Z. Naturforsch. 54b, 519—531 (1999); eingegangen am 20. November 1998 
  Published    1999 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0519.pdf 
 Identifier    ZNB-1999-54b-0519 
 Volume    54 
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