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Facet   section ZfN Section B:Volume 032  [X]
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1977 (337)
61Author    Requires cookie*
 Title    5N-NM R-U ntersuchim gen a n V erbindungen m it direkten N-N-Bindungen 15N N M R Studies on Compounds with Direct N-N Bonds  
 Abstract    H a r a l d S c h u l t h e i s s und E k k e h a r d F l u c k In s titu t fü r Anorganische Chemie der U niversität S tuttg art 15 N-15N Coupling Constants, 15N N M R 15N chemical shifts, the isotopic effect on chemical shifts and 1 J (15 N-15N) coupling constants of N a 2N 2C >3 , K.2SO3N 2O 2 , N a 2[CH2(N2 0 2)2], [(C2H 5)2N H 2][(C2H 5)2N N 2 0 2 ] and N 2O3 were measured. The discussion is based on a com pilation of reported 15N —l5N coupling constants. 
  Reference    (Z. Naturforsch. 32b, 257—264 [1977]; eingegangen am 9. Dezember 1976) 
  Published    1977 
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 Identifier    ZNB-1977-32b-0257 
 Volume    32 
62Author    Requires cookie*
 Title    Darstellung und Reaktionen des Tetramethylammonium  
 Abstract    -4.6-dimethyl-1.3.3.5.5-pentaoxo-l/J .f).3/6.5A6.2.4.6-perhydrotrithiatriazin-l-olats Preparation and Reactions of Tetram ethylamm onium-4,6-dim ethyl-l,3,3,5,5-pentaoxo-lA6,3A6,5A6,2,4,6-perhy drotrithiatriazin-1 -olat D i e c -La n g W a g n e r , H a r t m u t W a g n e r u n d O s k a r G l e m s e r Inorganic Heterocyclic Compounds Reaction of 2,4,6-trimethyl-l,l,3,3,5,o-hexaoxo-l A6 -,3A6 -,5A6 -,2,4,6-perhydrotrithiatria-zin, (CH3N S 0 2)3 (2), with trimethylamin forms a tetramethylammonium salt 
  Reference    (Z. Naturforsch. 32b, 265—267 [1977]; eingegangen am 29. September 1977) 
  Published    1977 
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 Identifier    ZNB-1977-32b-0265 
 Volume    32 
63Author    Requires cookie*
 Title    Röntgenographische Strukturuntersuchung von Cäsiumhexaoxo-tetrahydroxo-pentaborat-2-dimethylsulfoxid X-ray Study of the Structure of Cesiumhexaoxo-tetrahydroxo-pentaborate-2-dimethyl Sulfoxide  
 Abstract    The compound Cs[Bs0 6 (OH)4 ] • 2 DMSO was prepared by hydrolysis of tris(methoxy)-borane in organic solvents with small amounts of water in presence of cesium ierf-butylate and recrystallized in DMSO (dimethyl sulfoxide). Cs[Bs0 6 (0 H)4 ] • 2 DMSO crystallizes in the monoclinic space group P2i/a with a = 9.593(2), 6 = 19.179(4), c = 11.585(2) Ä, ß = 119.99(2)° and Z — 4. The crystal structure was determined by single-crystal diffracto­ meter data and refined to a conventional R value of 9.9%. The crystal structure consists of chains of pentaborate anions [Bs0 6 (OH)4 ]-linked by hydrogen bonds. The cesium cation and the DMSO molecules join the chains to sheets by coordination and hydrogen bonds respectively. 
  Reference    (Z. Naturforsch. 32b, 268—274 [1977]; eingegangen am 4. November/7. Dezember 1976) 
  Published    1977 
  Keywords    X-ray, Crystal Structure, Isopolyanions, Polyborates 
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 Identifier    ZNB-1977-32b-0268 
 Volume    32 
64Author    Requires cookie*
 Title    Kristall-und Molekülstruktur des Bis-tetraäthylammoniumtetracyanonitrosylferrat(I)  
 Abstract    Crystal and Molecular Structure of B is-tetraethylanunonium tetracyanonitrosylferrate(I) J ü r g e n K o p f u n d J ö r n S c h m i d t Tetracyanonitrosylferrate(I), Molecular Structure Crystals of [(CaHs^NMFe^NVjNO] are rhombic with a = 3392.0(21) [pm], b = 760.4(8) [pm], and c = 983.2(9) [pm]; the space group is Pna2i. The structure was determined by three-dimensional Patterson and Fourier methods on the basis of 1363 independent reflections. The unit cell consists of 4 molecular units. The anion forms a tetragonal pyramid which is only slightly distorted by narrowing one of the NC-Fe-NO angles. As expected from the electronic structure the apical NO group is almost linearly bonded to the central atom. The cations occur in two different conformations. 
  Reference    (Z. Naturforsch. 32b, 275—280 [1977]; eingegangen am 1. Dezember 1976) 
  Published    1977 
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 Identifier    ZNB-1977-32b-0275 
 Volume    32 
65Author    S.Requires cookie*
 Title    Strahlenchemische Cycloadditionen mit Äthylen und Acetylen (Produktbildung und Lösungsmittelwahl)  
 Abstract    R a d ia tio n Chemical C ycloaddition Reactions w ith Ethylene and Acetylene M a n f r e d J . M i r e a c h 1, M a r l i s F. M i r b a c h 1 u n d A l f o n s S a u The (2 + 2) cycloadditions of maleic acid anhydride (MSA) and 1,3-cyclohexadiene (CHD) to ethylene and acetylene were initiated with gamma-rays in different solvents. The four-membered ring products were formed with high selectivity and surprisingly high energy yields in solvents with triplett energies smaller than ethylene and acetylene but higher than MSA and CH D resp. In benzonitrile as a solvent MSA reacts with ethylene to give cyclobutane-l,2-dicarboxylic acid anhydride (1) (G = 0.04) and with acetylene to give cyclobut-3-ene-l,2-dicarboxylic acid anhydride (2) (G = 3.7). The cyclobutene derivative (2) is formed in >80% yield and the bicyclopropyl derivative (3), which is the main product in the photochemical reaction, with a yield of <20%. 1,3-Cyclohexadiene was also added to ethylene to give bicyclo(4,2,0)oct-2-ene (G = 0.4) and bicyclo(2,2,2)oct-2-ene (G = 0.1) under gamma irradiation in methylnaphthalene as a solvent. Under similar conditions addition to acetylene gave bicyclo(4,2,0)octa-2,7-diene (G = 0.04) and bicyclo(2,2,2)octa-2,5-diene (G = 0.3), respectively. 
  Reference    (Z. Naturforsch. 32b, 281—284 [1977]; eingegangen am 6. Oktober 1976) 
  Published    1977 
  Keywords    Cycloaddition, Ethylene, Acetylene, Maleic Acid Anhydride, 1, 3-Cyclohexadiene 
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 Identifier    ZNB-1977-32b-0281 
 Volume    32 
66Author    H. H. Zoorob, J. M. MichaelRequires cookie*
 Title    Michael Condensation Reactivity of 2-Cinnamoyl-5,6,7,8-tetrahydronaphthalene towards Acetylacetone, Ethyl Acetoacetate, Cyclohexanone and Malononitrile  
 Abstract    Acetylcyclohexenone, Indazole, Benzisoxazole, Carbazole The reactivity of 2-cinnamoyl-5,6,7,8-tetrahydronaphthalene (1) towards Michael condensation with acetylacetone, ethyl acetoacetate, cyclohexanone and malononitrile were studied. Also, the reaction of hydrazine hydrate, phenylhydrazine, hydroxylamine, with 2 were accomplished. Moreover, cyclization of 9 and 11 were performed. 
  Reference    (Z. Naturforsch. 32b, 289—292 [1977]; received August 27/November 22, 1976) 
  Published    1977 
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 Identifier    ZNB-1977-32b-0289 
 Volume    32 
67Author    Requires cookie*
 Title    Einfluß der Lebensdauer auf die Äthylen-Eliminierung aus Nichtterminalen Kohlenstoffpositionen bei Isomeren Cn H15+-Ionen in der Gasphase1 On the Influence of Life Time on the Ethylene Elim ination from Nonterm inal Carbon Positions of Isomeric Gaseous Cn H 15+ Ions  
 Abstract    F e r d i n a n d B o h l m a n n , M a n f r e d B r e h m u n d H e l m u t S c h w a r z Mass Spectrometry, Carbon Randomization, Carbenium Ions, Acetylenic Compounds Using 1 3 C-labelled compounds it is demonstrated that the extent of carbon randomiza­ tion preceding or accompanying the ethylene elimination from CnHi5 + is strongly in­ fluenced by the life tim e of the ions. Furtheron it is shown that the amount of these isomerisation reactions depends upon the structure o f the precursor ions. 
  Reference    (Z. Naturforsch. 32b, 293—295 [1977]; eingegangen am 29. November 1976) 
  Published    1977 
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 Identifier    ZNB-1977-32b-0293 
 Volume    32 
68Author    L. Szilágyi, P. H.Requires cookie*
 Title    A Convenient Route to N-Acetyl-D-glucosamine-2-C-d and N-Acetyl-D-m annosam ine-2-C-d  
 Abstract    Amino Sugars, C-Deuteration, X H NMR Title compounds were prepared through epimerisation o f 2-acetamido-2-deoxy-D-glucose in NaOD. The isotopic purity of the products was determined by NMR and mass spectroscopy. The mechanism of epimerisation is briefly discussed. 
  Reference    (Z. Naturforsch. 32b, 296—298 [1977]; received December 7 1976) 
  Published    1977 
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 Identifier    ZNB-1977-32b-0296 
 Volume    32 
69Author    Requires cookie*
 Title    Beiträge zur Chemie der Pyrrolpigmente, X V II1  
 Abstract    Struktur-und konformationsanalytische Untersuchungen am chromophoren System der Bilivioline [Biladiene-(a.b)] On the Chemistry of Pyrrole Pigments, X V II Investigations of Structure and Conformation of the Chromophoric System of Biliviolines [Biladienes-(a,b)] H e i n z F a l k , S t e f a n G e r g e l y , K a r l G r u b m a y r u n d O t m a r H o f e r The {Z,Z)-configuration of the bilivioline chromophoric system was established in ­ vestigating an appropriate model compound by means of pK measurement, X H NMR spectroscopy Lanthanide ion induced shift technique, electron absorption spectroscopy and P P P calculations. Moreover a syn-syn conformation which is twisted at the a-methine single bond and planar within the pyrromethene unit (based on the concept of partial structures of bile pigments) of the molecule was deduced. 
  Reference    (Z. Naturforsch. 32b, 299—303 [1977]; eingegangen am 12. November 1976) 
  Published    1977 
  Keywords    !H NMR, Lanthanide Shifts, PP P calculations, UV, Tautomeric Equilibrium 
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 Identifier    ZNB-1977-32b-0299 
 Volume    32 
70Author    Requires cookie*
 Title      
 Abstract    C U U -H 02 oxida­ tion a N=CH—Ar" n"2 . (Interm ediate A) Scheme I. tuted-benzimidazoles yields (cf. Table I). (6) are produced in good Ar-CH=C ,CN a) Ar b) Ar c) Ar d) Ar e) Ar f) Ar g) Ar h) Ar i) Ar j) Ar k) Ar I) Ar m) Ar I I) Ar 
  Reference    (Z. Naturforsch. 32b, 304 [1977]) 
  Published    1977 
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 Identifier    ZNB-1977-32b-0304 
 Volume    32 
71Author    Requires cookie*
 Title    Studies on 3,5-Diam ino Pyrazoles: Chemical Behavior o f 4-Phenylazo-3,5-diam inopyrazoles  
 Abstract    M o h a m e d H il m y E l n a g d i , E z z a t M o h a m e d K a n d e e l , a n d M o h a m e d R if a a t H a m z a E l m o g h a y a r Dethiocarbamoylation, Cyanoethylation, Pyrazolo[ 1,5-a]pyrimidines, Phenylazo Group Decoupling, NMR The behaviour of 3,5-diamino-4-phenylazopyrazole (1) toward isothiocyanates, acrylo-nitrile and ethyl ethoxymethylenecyanoacetate is investigated. An improved synthesis of 4-unsubstituted-3,5-diaminopyrazoles by an arylazo removal reaction is also reported. 
  Reference    (Z. Naturforsch. 32b, 307—310 [1977]; received August 20 1976) 
  Published    1977 
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 Identifier    ZNB-1977-32b-0307 
 Volume    32 
72Author    Requires cookie*
 Title    Pyrimidine Derivatives and Related Compounds, V Synthesis o f Some Isoxazolo [2,3-a] pyrimidines. A New Ring System  
 Abstract    M o h a m e d H i l m y E l n a g d i , E z z at M o h a m e d K a n d e e l , a n d K a m a l U s e f S a d e k Pyrimidine Derivatives, Isoxazolo[2,3-a]pyrimidines 3-Amino-5-phenyl-4-phenylazoisoxazole (1) reacts with ethyl acetoacetate to yield the corresponding ethyl isoxazolylaminocrotonate derivative (2) which could be thermally cyclized into the isoxazolopyrimidine derivative (4). On the other hand, condensation of 1 
  Reference    (Z. Naturforsch. 32b, 311—314 [1977]; received August 31 1976) 
  Published    1977 
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 Identifier    ZNB-1977-32b-0311 
 Volume    32 
73Author    Requires cookie*
 Title    Yields of 2-Deoxy-D-gluconic, D-Gluconic and Other Sugar Acids in Gamma-Irradiated Aqueous Solutions of D-Glucose  
 Abstract    H e r m a n n E s t e r b a u e r , J a c k S c h u b e r t , E d w a r d B. S a n d e r s , a n d Ch a r l e s C. S w e e l e y The yields of 2-deoxy-D-gluconic, D-gluconic and other sugar acids from 6 0 Co-gamma irradiated (dose rate = 4 Krads/min) D-glucose solutions are reported. The acids produced upon radiolyses were separated from glucose and neutral products by anion exchange, assayed by gas chromatography of the trim ethylsilyl derivatives, and definitive identification made by mass spectrometry. In He degassed, irradiated 0.055 M glucose G(2-deoxy-D-gluconic acid) = 0.62 and G(D-gluconic acid) = 0.20. The approximate G values for the other identified acids are: glyceric acid 0.03, 2-deoxy-tetronic acid 0.04, tetronic acid 0.03, 4-deoxypentonic acid 0.02, deoxyketogluconic acid 0.17. In N 20 saturated glucose solutions D-gluconic acid yields increased by a factor of ~ 1.9 while that of 2-deoxy-D-gluconic acid increased by a factor of only ~ 1.1. 
  Reference    (Z. Naturforsch. 32b, 315—320 [1977]; received October 29 1976) 
  Published    1977 
  Keywords    Irradiation, Glucose, Sugar Acids, 2-Deoxy-D-Gluconic Acid, D-Gluconic Acid 
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 Identifier    ZNB-1977-32b-0315 
 Volume    32 
74Author    G. S., M. K.Requires cookie*
 Title    Preparation of Spin-Labeled Phosphoroamidates in High Yield Using Imidazole as the Transfer Agent  
 Abstract    The spin-labeled (l-oxyl-2,2,6,6-tetramethyl-4-piperidyl)-phenyl imidazole-1-phos-phonate (4) was used to prepare (l-oxyl-2,2,6,6-tetramethyl-4-piperidyl)phenyl N-alkyl and N-aryl phosphoroamidates (8) in yields generally exceeding 70%. @ > -0 -P -N R 'R " ^ -0 -P -C I OR OR OR 4 8 1 0 Amidates 8 were also prepared from the corresponding chloridate 10. However, in the 
  Reference    (Z. Naturforsch. 32b, 321—327 [1977]; received September 3 1976) 
  Published    1977 
  Keywords    Spin-Labeled Phosphoroamidates, Amines, N itroxyl Moiety, Transphosphorylation 
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 Identifier    ZNB-1977-32b-0321 
 Volume    32 
75Author    G. S., M. K.Requires cookie*
 Title    Preparation of Triacetoneamine, I  
 Abstract    The preparation of triacetoneamine (1) by the condensation of acetone w ith ammonia in the presence of calcium chloride at room temperature is investigated. In addition to 1, acetonin (3), diacetone alcohol (4), m esityl oxide, and diacetoneamine (7) are formed during the reaction. The progress of the reaction is monitored by gas chromatography. The effects of the extent and the rate of stirring, the amount of ammonia introduced on the critical first day of the reaction, and the mesh size and the amount of calcium chloride on the purity and weight yield of 1 are studied. The yield of 1 is maximized by recovery of the unreacted acetone. The reaction at room temperature under optimized conditions is described. 
  Reference    (Z. Naturforsch. 32b, 328—337 [1977]; received November 29 1976) 
  Published    1977 
  Keywords    Triacetoneamine, Diacetoneamine, Mesityl Oxide, Acetonin, Diacetone Alcohol 
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 Identifier    ZNB-1977-32b-0328 
 Volume    32 
76Author    G. S., M. K.Requires cookie*
 Title    Preparation of Triacetoneamine, II  
 Abstract    The preparation of triacetoneamine (1) by the condensation o f acetone with ammonia in the presence of calcium chloride is investigated. The progress of the reaction is monitored by gas chromatography. The effects of added ammonium chloride, the total amount of ammonia introduced, and the temperature of the reaction on the weight yield and purity of 1 are investigated. The optimized conditions for the preparation of 1 at 59 °C are de­ scribed. 
  Reference    (Z. Naturforsch. 32b, 338—346 [1977]; received November 29 1976) 
  Published    1977 
  Keywords    Triacetoneamine, Diacetoneamine, Mesityl Oxide, Acetonin, Diacetone Alcohol 
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 Identifier    ZNB-1977-32b-0338 
 Volume    32 
77Author    Requires cookie*
 Title    Contributions to the Chemistry of Phosphorus, 711 About the Existence of Phosphorus Selenide Tribromide PSeBr3  
 Abstract    M a r i a n n e B ä u d l e r u n d B e r n d V o l l a n d In stitu t Phosphorus Selenide Tri bromide, Phosphorus Tri bromide, Selenium The title compound is formed in low concen­ tration by addition of selenium to PBr3 or by reaction of (CH3 Se)PBr2 with bromine. 
  Reference    (Z. Naturforsch. 32b, 347—348 [1977]; eingegangen am 26. November 1976) 
  Published    1977 
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 Volume    32 
78Author    Requires cookie*
 Title    IR Spectrum of Scandium Orthovanadate1  
 Abstract    M a r t a E . E s c o b a r und E n r i q u e J. B a r a n The infrared spectrum of ScYO4 is reported and discussed in comparison with those of YVO4 and of the lighter lanthanide ortho-vanadates. In order to facilitate the vibra­ tional assignment the spectra of a series of solid solutions of the type Sc(V0 4)i_w(P0 4)n are also measured and analyzed. 
  Reference    (Z. Naturforsch. 32b, 349—350 [1977]; eingegangen am 6. Dezember 1976) 
  Published    1977 
  Keywords    Scandium Orthovanadate, IR, Solid Solutions 
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 Volume    32 
79Author    Requires cookie*
 Title    Ternary Phases in the System Calcium-Nickel-Phosphorus  
 Abstract    A l b r e c h t M e w i s In stitu t Calcium Phosphides, Crystal Data, Nickel B y investigations in the system C a-N i-P we found two ternary phases. CaNii.95P2 crystallizes in a tetragonal lattice; a ThCr2 Si2 type structure is supposed. Ca2 .1N in .9P 7 crystallizes in a hexagonal lattice. 
  Reference    (Z. Naturforsch. 32b, 351—352 [1977]; eingegangen am 3. Dezember 1976) 
  Published    1977 
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 Volume    32 
80Author    Requires cookie*
 Title      
 Abstract    AB2 X 2 Compounds with the CaAl2Si2 Structure, I I 1 (A = C a; B = Zn, Cd; X = P, As) P e t e r K l ü f e r s u n d A l b r e c h t M e w i s In stitu t Four new ternary calcium compounds of zinc (cadmium) with a 5 B-element have been prepared. Analytic, pycnometric and X-ray powder data are given. The compounds are supposed to crystallize trigonally in a CaAl2 Si2-type structure. 
  Reference    (Z. Naturforsch. 32b, 353—354 [1977]; eingegangen am 3. Dezember 1976) 
  Published    1977 
  Keywords    Calcium Compounds, Zinc, Cadmium, 5 B-elements, Crystal Data 
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 Volume    32 
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