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1996 (12)
1Author    Rolf Minkwitz, Detlef KonikowskiRequires cookie*
 Title    Über verbesserte Darstellungs­ methoden für CF3OCH3 Improved Methods to Prepare CF3 O C H 3  
 Abstract    The reaction of CH 3I with CF3OCl at 203 K yields CF3O C H 3. The preparation of the ether by methylation of CsOCF3 with (CH3)2S 0 4 is also described. 
  Reference    Z. Naturforsch. 51b, 147—148 (1996); eingegangen am 21. Juni 1995 
  Published    1996 
  Keywords    1, 1, 1-Trifluoromethyl-methyl-ether, Preparation, N M R Spectra 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0147_n.pdf 
 Identifier    ZNB-1996-51b-0147_n 
 Volume    51 
2Author    Phosphonio-Substituted Tetrahydro-, -Diphosphinines, -Azaphosphinines, Georg Jochem, Martin Schm, HeinrichN. Öth ', Alfred SchmidpeterRequires cookie*
 Title    Phosphonio-substituierte Tetrahydro-l,3-diphosphinine un(j Tetrahy dro-1,2,6-azad i phospli in i ne  
 Abstract    The bis(triphenylphosphonio)propenide cation 1 provides two reactive CH sites in 1,3-position and can be condensed with the bis(dichlorophosphanyl)methylene triphenylphos-phorane 2 or the bis(dichlorophosphanyl)aniline 3 to form cationic six-membered rings: A tetrahydro-1,3-diphosphinine (4) with three phosphonio or phosphoranediyl substituents in 2,4,6-position and a tetrahydro-1,2,6-azadiphosphinine (5) carrying two such substituents in 3,5-position. The bromide of the latter was used for an X-ray structure analysis. The P111 ring members of the cations 4 and 5 can be oxidized in two steps by elemental sulfur to give the monothioxo and dithioxo derivatives 6. 7 and 8, 9. respectively. A crystal of the mixed chloride/bromide of 8 was used for another X-ray structure analysis. 
  Reference    Z. Naturforsch. 51b, 1761—1767 (1996); eingegangen am 16. August 1996 
  Published    1996 
  Keywords    Dichlorophosphanyl Ylides and Amines, Cyclocondensation, Phosphorus Heterocycles, 1, 3-Diphosphinines, 1, 2, 6-Azadiphosphinines 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1761.pdf 
 Identifier    ZNB-1996-51b-1761 
 Volume    51 
3Author    Michael Feist, Sergej Trojanov, Erhard KemnitzRequires cookie*
 Title    Die Kristallstrukturen von 1,4-Dimethylpiperazinium-tetrabromo- cobaltat(II) und -zinkat(II), (dmpipzH2) [Mn Br4] (M = Co, Zn)  
 Abstract    The Crystal Structures of 1,4-Dimethylpiperazinium Tetrabromocobaltate(II) and -Zincate(II), (dmpipzH2) [MHBr4] (M = Co, Zn) The compounds (dmpipzH2)[MnBr4] (M = Co, Zn) crystallize at room temperature from equi-molar solutions of 1,4-dimethylpiperazine and MBr2 • n H20 in 3M HBr. (dmpipzH2)[CoBr4] is isotypic with the homologous chlorometalates of Co and Zn and crystallizes in the mono­ clinic space group P2,/m with a = 6.424(3), b = 14.588(6), c = 7.102(6) A, ß = 90.87(6)°, Z = 2. (dmpipzH2)[ZnBr4], however, crystallizes in the monoclinic space group P2,/c with a = 7,605(5), b = 13,760(9), c = 13,286(7) Ä, ß = 93,03(6)°, Z = 4. Both structures con­ tain centrosymmetric cations (dmpipzH2)2+ in the chair form and slightly distorted tetrahedra [MBr4]2~ with a mirror plane in the case ofM = Co. Several distances N- • -Brin both structures are interpreted in terms of N-H- • Br hydrogen bonds which are favoured by the packing in the case of M = Zn. 
  Reference    (Z. Naturforsch. 51b, 9—13 [1996]; eingegangen am 12. Juni 1995) 
  Published    1996 
  Keywords    1, 4-Dimethylpiperazinium Tetrabromometalates(II), Cobalt, Zinc, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0009.pdf 
 Identifier    ZNB-1996-51b-0009 
 Volume    51 
4Author    Z. NaturforschRequires cookie*
 Title    Synthese und Dimerisierungsverhalten des l,l-Bis(trimethylsilyl)-2-(2,5-diisopropylphenyl)silens  
 Abstract    Tris(trim ethylsilyl)silylmagnesium bromide, (Me^SiX^SiMgBr, reacts with 2.5-diisopropyl-benzaldehyde to give 2,5-diisopropylphenyl-tris(trimethylsilyl)silylmethanol (1). With sodium 
  Reference    Z. Naturforsch. 51b, 370—3 (1996); eingegangen am 21. August 1995 
  Published    1996 
  Keywords    Silenes, Silene Dimerization, 2, 3-Disilanaphthalenes Tetrahydro, 1, 2-Disilacyclobutanes 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0370.pdf 
 Identifier    ZNB-1996-51b-0370 
 Volume    51 
5Author    JosephG. Robe, Duc Le Van, JostW. Innemöller, Bernt Krebs, M. Echtild LägeRequires cookie*
 Title    Reaktive E=C(p-p)7r-Systeme, XLIII [1] Darstellung und Charakterisierung P-Phosphino-oder P-Arsino-substituierter Fluorphosphaalkene des Typs R2E-P=C(F)NEt2 (R = Me, CF3, Me2N; E = P, As)  
 Abstract    Reactive E=C(p-p)-7r System s XLIII [1] Synthesis and Characterization o f P -Phosphino or P-A rsino Substituted Fluoro-phosphaalkenes of the Type R 2E -P=C (F)N Et2 (R = Me, C F 3, M e7N; E = R As) The easily accessible phosphaalkene HP=C(F)NEt2 (lb) reacts with halophosphanes or -arsanes R2EX (X = Cl, I) in the presence of NEt3 to give P-phosphino-or -P-arsino sub­ stituted fluorophosphaalkenes of the type RiE-P=C(F)NEti (2 -6) in high yields (60 -85 %) [R2E: (CF3)2P (2), Me2N(CF3)P (3), Me2P (4), (CF3)2As (5), M e2As (6)]. The analogous re-action of ib with CF3PI2 (molar ratio 1:2) unexpectedly leads to the triphosphetene Et2N 
  Reference    Z. Naturforsch. 51b, 778—784 (1996); eingegangen am 30. November 1995 
  Published    1996 
  Keywords    Phosphaalkenes, 1, 2, 3-Triphosphetenes, NMR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0778.pdf 
 Identifier    ZNB-1996-51b-0778 
 Volume    51 
6Author    Z. NaturforschRequires cookie*
 Title    ,1-Organoboration of Sterically Hindered Tetra-l-alkynylsilanes and the Crystal Structure of Tetrakis[l-(3,3-dimethyl)butynyl]silane  
 Abstract    Tetra-l-alkynylsilanes, Si(C sC R *)4 with R 1 = 'Bu (1) and SiMe3 (2) react with triethyl-borane, E t3B. by intermolecular 1,1-ethyloboration followed by intramolecular 1.1-vinylo-boration. to give the substituted siloles 3 and 5 with two R 'C = C groups linked to silicon. The formation of 5 (R 1 = SiMe3) requires exactly one equivalent of E t3B, whereas 3 (R 1 = 'Bu) is formed after = 2 0 d in boiling toluene in the presence of a large excess of E t3B, and the remaining 'B u -C = C groups in 3 do not react with E t3B. The 1,1-organoboration of 2 using one equivalent of 9-ethyl-9-borabicyclo[3.3.1]nonane, Et-9-BBN, proceeds similar to the E t3B-reaction, to give mainly the silole derivative 6, in which the bicyclic ring system is enlarged by two carbon atoms. This product is the result of a kinetically controlled reaction. The single crystal X-ray analysis of 1 has been carried out (space group Pnm a; a = 990.0(2), b = 1668.0(3), c = 1479.0(3) pm), and its crystal structure is com pared with that of the corre­ sponding tin compound 1 (Sn). 
  Reference    Z. Naturforsch. 51b, 1320—1324 (1996); received March 14 1996 
  Published    1996 
  Keywords    Tetra-l-alkynylsilanes, 1, 1-Organoboration, Siloles, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1320.pdf 
 Identifier    ZNB-1996-51b-1320 
 Volume    51 
7Author    G. Erhard, H. Enesa, A. Nton Rieker, M. Arkus, N. Eum Ayerb, W. Olfgang HillerRequires cookie*
 Title    ,4-Addition of Lithium Organyls to /?ara-Quinols / Structure Determination of 2,6-Di-te/t-butyl-4-hydroxy-4,5-diphenyIcyclohex-2-en-l-one  
 Abstract    Addition of lithium organyls to sterically hindered para-quinols leads to 1,2-or 1,4-adducts. The 1,4-addition prevails, if the 4-substituents in the quinol and the organic group in the lithium organyl are large. Four 1,4-addition products (2-cyclohex-2-en-l-ones) are synthesized and their structures investigated by NMR spectroscopy. The aryl groups at C-4 and C-5 acquire equatorial positions, the alkyl group at C-6 is bisectional. These results are confirmed by X-ray analysis of 2,6-di-terr-butyl-4-hydroxy-4,5-diphenylcyclohex-2-en-1 -one, revealing a twist boat conformation of the cyclohexene ring. 
  Reference    Z. Naturforsch. 51b, 381—387 (1996); received August 11 1995 
  Published    1996 
  Keywords    Crystal Structure, Quinol, 1, 4-Addition, Lithium Organyl, Cyclohex-2-en-l-ones 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0381.pdf 
 Identifier    ZNB-1996-51b-0381 
 Volume    51 
8Author    H. Möhrle, U. Von Der Lieck-WaldheimRequires cookie*
 Title    Vinamidinium-Salze als Nucleophile Vinamidinium Salts as N ucleophiles  
 Abstract    1,4-diazepinium salts could not be aminomethylated with conventional methods, but the hydrochlorides produced with methyleniminium salts the C-Mannich-compounds. The reactivity of the substrate was mainly controlled by electronic effects of the substituents. Aminomethylation of 1,5-diazapentadienium salts occurred only if the conformations caused no steric hindrance of the ß-C-atom. Methyl substituted 2,3-dihydro-1,4-diazepinium salts reacted with 1,3,5 triazine to pyrimidine anellated derivatives. 
  Reference    Z. Naturforsch. 51b, 421—430 (1996); eingegangen am 4. Juli 1995 
  Published    1996 
  Keywords    Mannich Reaction, Iminium Salts, 1, 3, 5 Triazine, Push-Pull-Systems 2, 3-Dihydro- 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0421.pdf 
 Identifier    ZNB-1996-51b-0421 
 Volume    51 
9Author    P.Requires cookie*
 Title    Phosphonio-substituierte 1,3-Diphosphanaph thaline aus der a,o-Kondensation von Phosphonium-benzyliden  
 Abstract    h o sp h o n io -S u b stitu te d 1 .3 -D ip h o sp h a n ap h th a le n es from th e a,o -C o n d e n sa tio n o f P h o sp h o n iu m -b en z y lid e s G eo rg Jo ch em , A lfred S chm idpeter* 
  Reference    Z. Naturforsch. 51b, 773—777 (1996); eingegangen am 21. Dezember 1995 
  Published    1996 
  Keywords    Phosphonium Ylides, Electrophilic Aromatic Substitution, 1, 3-Benzodiphosphinines, Spontaneous Chlorophosphine Dissociation, Selective Oxidation by Elemental Sulfur 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0773.pdf 
 Identifier    ZNB-1996-51b-0773 
 Volume    51 
10Author    B. Ernd, W. Rackm Eyer, D. Örfler, W. Olfgang Milius, M. Ax, H. ErberholdRequires cookie*
 Title    ,1-Organoboration of Trimethyl-l-propynyltin Using Diorganoboryl-Substituted Ferrocenes  
 Abstract    The reactions of various diorganoborylferrocenes, F c -B R 2 [1, R = Me (a), Et (b), 'Pr (c), 'Bu (d), Ph (f), R2B = 9-borabicyclo[3.3.1]nonyl (e)] and 1,1 '-bis(9-borabicyclo[3.3.1]nonyl)-ferrocene (2) with trimethyl-l-propynyltin (3) were studied, and the products of the 1,1-organoboration were characterized as the alkenyltin compounds 4 -6 by 'H, UB, 13C and 119Sn NMR. In the cases of l a -I d and If, there is competition between the transfer of a ferrocenyl group and the other organyl groups R from boron to carbon, whereas in the case of the 9-borabicyclo[3.3.1]nonane derivatives le and 2, the enlargement of the bicyclic system takes place selectively (compounds 4e and 6). The molecular structure of the product 6, obtained from the reaction between the l,l'-diborylated ferrocene 2 and two equivalents of 3, was determined by single crystal X-ray analysis (space group P2x!c\ monoclinic; Z = 4, a = 958.3(2), b = 1610.4(3), c = 2405.3(5) pm and ß = 90.33(3)°). 
  Reference    Z. Naturforsch. 51b, 851 (1996); received October 26. 1995 
  Published    1996 
  Keywords    Ferrocenes, Trimethyl-l-propynyltin, 1, 1-Organoboration, Alkenyltin Compounds, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0851.pdf 
 Identifier    ZNB-1996-51b-0851 
 Volume    51 
11Author    Z. NaturforschRequires cookie*
 Title    Elektronentransfer und Ionenpaar-Bildung  
 Abstract    , 47 [1] Titrationen von 1,2,4,5-Tetracyanbenzol und 7,7,8,8-Tetracyan-/;-chino-dimethan mit Natriummetall in aprotischen Lösungen E le ctro n T ran sfer an d Ion P air F o rm atio n , 47 [ 1 ] T itratio n s o f 1,2 ,4 ,5 -T etracy an o b en zen e and 7 ,7 ,8 ,8 -T etracy an o -/?-q u in o d im eth an e w ith S o d iu m M etal in A p ro tic S o lu tio n s H an s B ock*, M a rk u s K leine 
  Reference    Z. Naturforsch. 51b, 1215—1221 (1996); eingegangen am 25. Januar 1996 
  Published    1996 
  Keywords    1, 2, 4, 5-Tetracyanobenzene, 7, 7, 8, 8-Tetracyano-/?-quinodimethane, Sodium Metal Reduction, UV/VIS Spectra 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1215.pdf 
 Identifier    ZNB-1996-51b-1215 
 Volume    51 
12Author    VasilyRequires cookie*
 Title    Chemistry of the l,3>5-Triaza-2-phosphorin-4,6-diones, Part XII*. Synthesis and Characterization of 2-PhenyI-2-(/?-tolylthio)-l,3?5- trimethyI-l,3,5-triaza-4,6-dione-2-phosphorinonium Salts  
 Abstract    A . P in ch u k , Io n N e d a , C h ristian M üller, H o lg e r T h ö n n e ss e n , P e te r G. Jones, R e in h a rd S chm utzler The reaction of l,5-bis(trimethylsilyl)-l,3.5-trimethylbiuret (1) with/M olylsulfenyl chloride (2) furnished l-(/?-tolylthio)-5-trimethylsilyl-l,3,5-trimethylbiuret (3). In the reaction of 3 with phenyldichlorophosphine, 2-phenyl-2-(/?-tolylthio)-l,3,5-trimethyl-l,3,5-triaza-4,6-dione-2-phosphorinonium chloride (4) was formed. The same product was obtained from the reac­ tion of 2-phenyl-l,3,5-trimethyl-l,3,5-triaza-2/.3-phosphorin-4,6-dione (6) with p-tolylsulfenyl chloride (2). Compound 4 was isolated and characterized in the form of the hexachloroanti-m onate (4a). The spirophosphorane 2-phenyl-l,3,5-trimethyl-l,3,5-triaza-7,10-dioxa-8,9-perchlorobenzo-2As-phosphaspiro-[4.5]decan-4,6-dione (7) was prepared by the reaction of 4 with tetrachloroorthobenzoquinone. The new products were characterized by 'H -and 13C NMR spectroscopy, elemental analysis, 31P NMR spectroscopy in the case of 4a. 6 and 7, and mass spectrometry (4a). Single-crystal X-ray structural analyses of compounds 4a and 7 were conducted. The phosphorus atom of 4a has the expected tetrahedral geometry, with a rather short P-S bond of 204.9(2) pm. In 7 the geometry at phosphorus is almost ideal trigonal bipyramidal. Weak hydrogen bonds are formed from a C (:0) group to deuterochloroform of solvation. 
  Reference    Z. Naturforsch. 51b, 1494—1500 (1996); received February 13 1996 
  Published    1996 
  Keywords    1, 3, 5-Trimethyl-Substituted 1, 3, 5-Triaza-4, 6-dione-2-phosphorinonium Derivatives, Intram olecular Rearrangem ent, NMR Spectra, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1494.pdf 
 Identifier    ZNB-1996-51b-1494 
 Volume    51