bluuebunny/crossref_metadata_2025 huggingface dataset:
NOTIZEN: Hinweise auf die Existenz von Trimethylsilylmagnesiumverbindungen / Evidence for the Existence of Trimethylsilylmagnesium Compounds
Authors: Rösch Lutz , Erb Wolfgang , Müller Hartwig
Published: March 2015

Trimethylchlorosilane reacts with magnesium in hexamethylphosphortriamide yielding hexamethyldisilane. An organosilylmagnesium compound is proposed as reactive intermediate in this reaction. Further evidence for the existence of trimethylsilylmagnesium compounds could be obtained in the reaction of trimethylchlorosilane with highly reactive magnesium in tetrahydrofurane as solvent.
Notizen: Reduction of Indolic Imides with Sodium Borohydride
Authors: Rahman Atta-Ur , Waheed Nighat
Published: March 2015

The reduction of imides with sodium borohydride affords ring cleaved products instead of the corresponding carbinol lactams suggested previously.
Massenspektrometrische Untersuchungen an Borchelaten, III. Massenspektrometrische Fragmentierung von Fluorobor- und Phenylborchelaten.
Authors: Hohaus Eberhard , Riepe Wolfgang
Published: March 2015

Mass spectra of several fluoroboron and phenylboron chelates were compared with regard to the influence of the boron substituent F and C6H5.

The fragmentation pattern depends very strongly on the type of the substituent.

In the case of the fluorine substituent, the three bonding states of boron will be reached preferably by opening the chelate ring. For the substituent C6H5 this state of boron will be reached by elimination of C6H5.
Reactions with 2-Phenylhydrazono-4-thiazolidinone and its Derivatives
Authors: Kassab Nazmi Abd Elatif , Alla Sanaa Osman Abd , Ead Hamed Abdel Reheem
Published: March 2015

2-Phenylhydrazono-4-thiazolidinone (1) and its 5-substituted derivatives (4) and (6) were cyclized by formaldehyde or aromatic aldehydes to afford the corresponding 2-phenyl-tetrahydrothiazolo[2,3-c]-1,2,4-triazol-5-ones (2, 3) and (7). Compounds 3 were also obtained by the action of aromatic aldehyde on 2-phenyltetrahydrothiazolo[2,3-c]-l2,4-triazol-5-one (2).
Notizen: Synthesis of Some ω,ω′-Bis(diguanido-oxy)Alkanes
Authors: Suresh K. S. , Malkani R. K.
Published: March 2015

Synthesis of a few bis(diguanido-oxy)-alkanes which are likely to possess good bacteriostatic properties have been reported.
Darstellung und Eigenschaften von Ca2AsBr, Sr2AsCl und Ca3AsBr3.
Authors: Hadenfeldt Claus
Published: March 2015

Dark-brown Ca2AsBr and yellow-green Ca3AsBr3 were prepared by reaction of Ca, As, and CaBr2 at 900-1000°C and 760-800°C resp., dark-violet Sr2AsCl from Sr, As, and SrCl2 at 900-1000°C. Ca2AsBr possesses an extended homogeneity range (Ca2AsBr to Ca2.5AsBr2), Sr2AsCl only a narrow one; Ca3AsBr3 is a stoichiometric compound. In contrary to Ca2AsBr Ca3AsBr3 is not stable at 1000°C. Analytical results, densities, and lattice constants of the phases are given.
Reaktion von 1.4-Dienen mit Metallkomplexen, I Darstellung und Röntgenstrukturanalyse eines π-enyl-Komplexes der Zusammensetzung (C8H13PdCl)2/ Reaction of 1,4-Dienes with Metal Complexes, I Synthesis and X-ray Structure Determination of a π-enyl Complex of Composition (C8H18PdCl)2
Authors: Feldhaus Peter , Ratka Richard , Schmid Hermann , Ziegler Manfred L.
Published: March 2015

Reaction of (C6H5CN)2PdCl2 and 1,3-dimethylenecyclohexane led to an exocyclic π-enyl complex of formula (C8H13PdCl)2-bis(η3-2-methylene-6-methylcyclohexyl)(di-µ-chloro)-dipalladium. IR and 1H NMR data are in agreement with this formulation.

The compound is monoclinic, with unit cell dimensions α = 499.97 ± 0.08, b =1342.26 ± 0.19, c =1379.60 ± 0.20 pm, β = 99.43 ± 0.02°, space group C5h
2-P21/C, Ζ = 2, dX-ray = 1.83 g/cm3.

The structure was determined from three-dimensional X-ray data by Patterson and Fourier methods. Least squares refinement by use of 1045 independent reflections has reached R1 = 5.6%.
Mechanismus und Kinetik der Zersetzung von Methan-Wasser-Gemischen im kalten Plasma.
Authors: Simionescu Cr. I. , Dumitriu S. , Popa V. I.
Published: March 2015

In the present paper the mechanism and kinetics of methane-water mixtures decomposition in cold plasma are discussed. It was found that nature and composition of the products depend on reaction time, ratio of the two components, and how long the products are in contact after the decomposition was performed.

Reactions in the decomposition system generally follow two mechanisms: corresponding to the discharge phase and to postreaction one. The highest yield of formaldehyde was obtained for the ratio methane water of 0.6-1 and two minutes of discharge.
Notizen: Einige neue ternäre Goldchalkogenide/ Some New Ternary Gold Chalcogenides
Authors: Blachnik Roger , Gather Bernd
Published: March 2015

The ternary compounds Au2As2Te3, AuSbTe und AuSb0,077Te2 have been found. Melting point or peritectic temperature as well as microhardness and X-ray diagramm have been measured.
Notizen: Hochdruckreaktionen, ΧII / High Pressure Reactions, XII
Authors: Proetzsch R. , Bieniek D. , Korte F.
Published: March 2015

γ-Thiovalerolactone (1), under high pressure (15 kbar, 170°C), forms the compounds 2 and 3. Under similar conditions, δ-thiovalerolactone polymerizes nearly quantitatively; at 11 kbar and 170°C, 5 is formed in 2% yield. Thiooxindole 7 reacts to yield 8 and the thermically very stable trimer 9.
Notizen: Triphenylmethylradikale durch inverse Stevens-Umlagerung.
Authors: Bölsing F. , Spanuth E.
Published: March 2015

Diphenyldiazomethane reacts with triphenylborane to yield benzophenonazine and benzophenone triphenylmethylhydrazone. The formation of the latter is elucidated by ESR spectroscopic detection of the triphenylmethyl radical. The reaction can be modified to a simple method for the preparation of triphenylmethyl radicals in high yields.
Synthese und Photolyse von 5-Diazo-5-[13C] -homoadamantanon-(4).
Authors: Zeller Klaus-Peter
Published: March 2015

The synthesis of 5-diazo-5-[13C]-homoadamantan-4-one (12) is achieved by ring expansion of adamantanone with 13C-labelled diazomethane, conversion of the resulting 4-[13C]-homoadamantan-4-one (10) to the hydroxymethylene compound (11), followed by deformylative diazo group transfer reaction. The photolysis of 12 with pyrex filtered UV-light in dioxane-water (10:1) yields adamantan-2-carboxylic acid containing all the label in the 2-position of the adamantane skeleton. The total absence of isotope scrambling excludes the intermediate formation of the polycyclic oxiren (16) (Scheme 3).
Sesquiterpenester der Α-Reihe aus Euonymus europaeus L.1.
Authors: Römer Axel , Thomas Hartmut , Budzikiewicz Herbert
Published: March 2015

The structure of 6 esters of 7 β-hydroxy-3,4-didesoxy-8-epi-maytol has been elucidated.
Phosphorus Compounds with the VI B Group Elements
Authors: Monteil Y. , Vincent H.
Published: March 2015

The preparation and the properties of phosphorus sulfides and selenides are reviewed.

The exact number of phosphorus sulfides and selenides has been determined from the phase diagram. Phosphorus does not react with tellurium. The ternary diagram P—S—Se shows no P—S—Se compounds. The domains of P—S and P—Se glasses has been also determined. IR and mass spectrometry show that phosphorus sulfides and selenides have a tetrahedral arrangement of P atoms close to that of white phosphorus.
Notizen: Die Kristallstruktur von Dy2Se3.
Authors: Range Klaus-Jürgen , Leeb Richard
Published: March 2015

The U2S3-type structure of Dy2Se3 was confirmed and refined from single-crystal data.
Notizen: Darstellung von H3[Mn(CN)5NO] und H3[Cr(CN)5NO] und ihrer Ammoniumsalze.
Authors: Mohai B. , Horváth A.
Published: March 2015

The carmine-red H3[Mn(CN)5NO] and the olive-green H3[Cr(CN)5NO] were prepared in crystalline form by the acid treatment of the corresponding potassium compounds, and the ammonium salts of these by neutralizing the solutions of the above acids.
Die Hydrolyse einiger Borsäureester unter Base-Einfluß in nichtwäßrigen Lösungsmitteln / The Hydrolysis of Some Tris(organyloxy)boranes under Alkaline Influence in Non-aqueous Solvents
Authors: Heller G. , Ross H.
Published: March 2015

The hydrolysis of tris(organyloxy)boranes (boric acid esters) in organic solvents in the presence of KOH leading to potassium polyborates (free from water of crystallization) is studied as to the influences of (a) the reaction medium (ethanol or ligroine/ethanol), (b) the concentration of water, (c) the organyl group of the boric acid ester (methyl, isopropyl, or phenyl), (d) the time of stay of the precipitated insoluble polyborates under the mother liquor (15 to 61850 s), and (e) the temperature during precipitation and the time of stay (—18 to + 60°C).

In the first stage of the reaction, during precipitation time, ester hydrolysis is followed by condensation, while aggregation and desorption processes occur between the time of precipitation and filtration.
Ein gemischt methyl/phenyl-substituiertes Carbodiphosphoran. Darstellung, Reaktionen und verwandte Verbindungen / A Mixed Methyl-/Phenyl-substituted Carbodiphosphorane. Synthesis, Reactions, and Related Compounds
Authors: Hussain M. Sakhawat , Schmidbaur Hubert
Published: March 2015

From the reaction of bis-diphenylphosphino-methane and methyl bromide a diquaternized onium salt is obtained, which is converted into the carbodiphosphorane MePh2P=C=PPh2Me by sodium amide in THF. This bis-ylide was characterized by its reactions and its NMR spectra. With methyl chloride, the above diphosphine yielded the phosphino-phosphonium salt, which forms a phosphino-ylide upon dehydrohalogenation.
Untersuchung der cis-trans-Isomerisierung in Bis(5.5-dimethyl-2-hexenyl)-zink mittels kernmagnetischer Sättigung / A Nuclear Magnetic Saturation Study of the cis-trans Isomerization in Bis(5,5-dimethyl-2-hexenyl)-zinc
Authors: Bausch R.
Published: March 2015

Kinetic parameters of the cis-trans isomerization in bis(5,5-dimethyl-2-hexenyl)-zinc have been determined by means of nuclear magnetic saturation transfer. Novel methods for the acquisition and analysis of saturation data are reported. The results are consistent with a dynamic allylic system passing through the secondary metal alkenyl form as an intermediate in the equilibrium of cis-trans isomers.
Zur Elektronenstruktur metallorganischer Komplexe der f-Elemente, IV Zuordnung der Absorptionsbanden im Raumtemperatur-Absorptionsspektrum von Tris-(cyclopentadienyl)-uran(IV)-tetrahydroborat / The Electronic Structure of Organometallic Complexes Involving f-Electrons, IV Assignment of the Absorption Bands in the Room Temperature Absorption Spectrum of Tris-(cyclopentadienide)-uran(IV)-borohydride
Authors: Ambergeb H.-D. , Sienel G. R.
Published: March 2015

The bands of the room temperature absorption spectrum of (C5H5)3U(IV)BH4 have been identified on the basis of the complete energy matrix of the tetrahedral f2-system. Using the parameter set: F2 = 181, F4 = 33.5, F6 = 3.8, ζ5f = 1815, B4° = —495 and B6° = —292 cm-1 a good agreement between observed and calculated signals has been achieved.
Austauschreaktionen an komplexgebundenen Liganden von Elementen der V. Hauptgruppe, V1 Darstellung und Reaktionen von Komplexen des Typs π-C5H5Mn(CO)2L (L = Phosphid, Amid) / Exchange Reactions at Complexed Ligands of Elements of Group V B1 / Preparation and Reactions of Complexes of the Type π-C5H5Mn(CO)2L (L = phosphide, amide)
Authors: Höfler Mathias , Hausmann Heinz , Saal Wilhelm
Published: March 2015

The reduction of the complexes C5H5Mn(CO)2L (L=P(C6H5)2Cl, P(C6H5)(Et)Cl and P(C6H5)Cl2) with Na in liquid NH3 yields the complexes C5H5Mn(CO)2L′ (L′=P(C6H5)2Na, P(C6H5)(Et)Na and P(C6H5)Na2).

The reaction of these complexes with CH3J and of CpMn(CO)2PØ2Na with H2O, CH2Cl2, CCl4, J2 and CH3COCl are described. Furthermore it has been found, that n-butyl-lithium yields C5H5Mn(CO)2NMe2Li if reacted with C5H5Mn(CO)2NMe2H.
Notizen: Silydianin und Silychristin, zwei isomere Silymarine aus Silybum marianum L. Gaertn. (Mariendistel) / Silydianin and Silychristin, two Isomeric Silymarins from Silybum marianum L. Gaertn. (milk thistle)
Authors: Wagner H. , Seligmann O. , Seitz M. , Abraham D. , Sonnenbichler J.
Published: March 2015

Two isomeric flavonolignans (Silymarins) have been isolated from the fruits of Silybum marianum L. Gaertn. and structurally elucidated mainly by means of NMR/mass spectroscopy and X-ray analysis respectively.
Preparation and Characterization of Silicon(IV) Formate
Authors: Paul Ram Chand , Puri Tripta , Kapoor R.
Published: March 2015

Silicon(IV) formate has been prepared by the reaction of silicon(IV) chloride and anhydrous formic acid. The compound has been characterized by elemental analyses, thermogravimetry and infrared spectral data.
Adsorption von Aceton an Magnesiumoxid.
Authors: Koubowetz Franz , Noller Heinrich , Latzel Johannes
Published: March 2015

The adsorption of acetone on MgO was studied by IR spectroscopy, the desorption products were analyzed with a mass spectrometer. Furthermore, the heat of adsorption and the coverage of the surface were calculated from adsorption isothermes measured at various temperatures.

Acetone is adsorbed over (weak) hydrogen bonds to surface hydroxyl groups as well as coordinatively bound to the cation Mg2+. This bonding to the cations causes strong shifts of the carbonyl band (up to 100 cm-1) and the CH3 bands (Δν≈55 cm-1) to lower wavenumbers. At 120°C, desorption of acetone, and at 320°C and 400°C of methane is detected. Using d6-acetone or D2O, the methane observed can be shown to be formed from hydrogen of acetone rather than with participation of hydrogen of surface hydroxyl groups.
Über Galvinole und Galvinoxyle, II EPR-HFS- und elektronen-spektroskopische Untersuchung von Galvinoxyl-Mehrspinsystemen.
Authors: Gierke W. , Harrer W. , Kibste B. , Kurreck H. , Reusch J.
Published: March 2015

The synthesis of several so far unknown mono- and oligo-galvinols and galvinoxyls is described. The ESR hyperfine splitting measurements in liquid solution indicate that the spin exchange frequency is greater than the hyperfine splitting in the galvinoxyl biradicals (J≫a). The electronic absorption spectra of the galvinols and galvinoxyls are discussed taking into account the different prototropic and redox equilibria, respectively. Using magnetic susceptibility measurements the singlet-triplet and doublet-quartet splitting is studied.
Säurekatalysierte Umlagerungen von 1.5-Cyclo-2-keto-steroiden.
Authors: Habermehl Gerhard , Walz Wolfgang
Published: March 2015

With 98% formic acid 1,5-cyclo-10α-cholestan-2-on (5) is isomerized to yield 19-nor-5α- methyl-Δ1.(10)-cholesten-2-on (6). Reaction of 5 with BF3 in benzene yielded mainly 6; as by-product des-A,B-nor-10-3'(2'-cyclopentane-1'-on)-cholestane (8) was obtained. On reaction of 5 with FeCl3 • 6 H2O in absolute methanol or ethanol 5 α-methoxy-, or 5 α- ethoxy-10 a-cholestan-2-one (18, resp. 14) was formed.
Metallocenylborane, IV. Diborylverbindungen des Ferrocens und Cymantrens.
Authors: Ruf Werner , Renk Thomas , Siebert Walter
Published: March 2015

Ferrocene reacts with BI3 and BBr3 to give 1,1′-bis(dihalogenboryl)ferrocenes; the cyclopentadienylring in cymantrene is twice borylated by BI3. By halogen exchange with AsF3 and AsCl3, by methylation with Sn(CH3)4, by cleavage of (C2H5)2O, by redox reaction with (CH3S)2 and by reaction with (C2H5)2NH the corresponding diborylferrocenes are obtained. The air-sensitive halogenborylferrocenes form donor-acceptor compounds with Lewis bases. 1H, 11B and 13C NMR data reflect increasing π-acceptor properties with increasing Lewis acidity of the boryl groups.
Neue intermetallische Verbindungen im anti-PbFCl-Strukturtyp.
Authors: Dörrscheidt Wolfgang , Schäfer Herbert
Published: March 2015

Three new intermetallic compounds CaMnGe, SrMnGe and BaMnGe have been prepared. They crystallize tetragonal in the anti-PbFCl-structure type with the following constants :

CaMnGe: a = 4.23(1); c = 7.27(1); c/a = 1.72,

SrMnGe: a = 4.40(1); c = 7.52(1); c/a = 1.71,

BaMnGe: a = 4.50(1); c = 7.92(1); c/a = 1.76.
Vier- und fünfgliedrige Phosphorheterocyclen, XIV Kationen des hexakoordinierten Phosphors.
Authors: Schmidpeter Alfred , Criegern Thomas Von , Blanck Klaus
Published: March 2015

The spirobi(benzodioxaphosphole) system stabilizes high phosphorus coordination. Thus bis(o-phenylenedioxy)chlorophosphorane adds pyridine in a fast first step without dissociation to a neutral, and in a slower second step to a cationic hexacoordinate phosphorus species. The equilibria compositions were determined by 31P NMR. The cation of the bis(pyridine) adduct can be isolated as the stable crystalline chloride which partly decomposes on dissolving. More stable, even in boiling water, is the cation of the 2,2′-bipyridine adduct.

1H NMR studies of the bis(pyridine) adduct lead to a cis structure. A δ31P comparison for hexacoordinate spirobi(benzodioxaphospholes) is given.
The Comparative Photochemical Behaviour of Dibenzenechromium and Benzenetricarbonyl Chromium
Authors: Gilbert Andrew , Kelly John M. , Budzwait Marion , Von Gustorf Ernst Koerner
Published: March 2015

In comparison with (C6H6)Cr(CO)3, (C6H6)2Cr is relatively light stable. The major part of the light energy absorbed by (C6H6)2Cr leads neither to its decomposition or ligand exchange, nor can it be transferred to common low energy triplet acceptors. Internal dissipation of energy, either by rapid conversion to the ground state or by rapid reversible isomerization, must be an important process.

In the case of (C6H6)Cr(CO)3, the main pathway to the previously reported lightinduced exchange of benzene involves an intermediate which is suggested to be (benzene)-dicarbonylchromium (1) and not a one-step dissociation of the excited molecule, to give Cr(CO)3 and benzene1b: 1 is also of major importance for the exchange of CO.
Die Kristallstruktur des Silber-N-cyclohexylamidoperchlorats.
Authors: Pritzkow H.
Published: March 2015

Silver-N-cyclohexylamidoperchlorate crystallizes in the monoclinic space group P21/n with the cell parameters a = 12.810 A, b= 24.710 Å, c= 6.051 Å, β= 90.0°. The crystal structure is built up by —N—Ag—N—Ag-chains. The N—Cl distance is much longer than in K2NClO3, but slightly shorter than in other compounds with N—Cl bonds.
Polarisations-absorptionsspektrometrische Untersuchungen zur elektronischen und geometrischen Struktur der Oktacyanokomplexe des Molybdäns und Wolframs, I Das Mo(CN)8 -Ion in K4Mo(CN)8 · 2 H2O / Polarization-Absorption Spectrometric Studies of the Electronic and Geometrical Structure of the Octacyano Complexes of Molybdenum and Tungsten, I The Mo(CN)8 Ion in K4Mo(CN)8 · 2 H2O
Authors: Morys P. , Gliemann G.
Published: March 2015

Polarized absorption spectra of the ions Mo(CN)8
4- and W(CN)8
4- were measured on single crystals of the compounds K4Mo(CN)8 · 2 H2O and K4W(CN)8 · 2 H2O over the spectral region 10-47 kK and at temperatures from 300°K to 4.2°K. The results obtained were interpreted on the basis of the ligand field theory.

According to their d → d-spectrum, these complex ions in the crystalline state have a quasi-dodecahedral coordination structure with the exact symmetry D2. The deviation from the ideal dodecahedral structure is appreciably smaller at low temperatures than at room temperature.

Contrary to the results of earlier X-ray structure determinations, the only space group which can be assigned to the crystals of K4Mo(CN)8 · 2 H2O and K4W(CN)8 · 2 H2O is C9
2v.
Notizen: Der Mößbauereffekt an Nitrokomplexen AI
2PbFe(NO2)6 [AI: Κ, Tl, Rb, Cs] mit low-spin-konfigurierten Fe2+-Ionen.
Authors: Peeler J. , Backes G. , Schmidt K. , Reinen D.
Published: March 2015

Mössbauer data of low spin Fe2+-ions in nitro complexes AI
2PbFe(NO2)6 [AI: K, Tl, Rb, Cs] are presented. Explicitly the dependence of the isomer shift δ on the FeN bond length is studied and correlated with the ligand field parameters Δ of the corresponding Ni2+- and Cu2+-compounds.
Beiträge zur Chemie des Phosphors, 68 Tri-t-butyl-cyclotriphosphan.
Authors: Baudler Marianne , Hahn Josef , Dietsch Hermann , Fürstenberg Gabriele
Published: March 2015

In the reaction of magnesium with trimethylchlorosilane and t-butyldichlorophosphane the hitherto unknown tri-t-butyl-cyclotriphosphane, (t-BuP)3 (1), is produced besides the partially silylated phosphanes t-BuP(SiMe3)2 and (t-BuPSiMe3)2 as well as the cyclotetraphosphane (t-BuP)4. Shortly after the beginning of the reaction the amount of 1 is about 50 mole-% and decreases during the reaction time. Thermally and in solution the P3 ring compound (1) is surprisingly stable and can be isolated in a pure state by fractional distillation. (t-BuP)3 clearly differs from the oligomeric (t-BuP)4 by the lower melting point, the molar mass and by the 31P NMR and IR spectra. The t-butyl groups in 1 are situated above and below the P3 ring plane.
Gemischtligandkomplexe von Osmium(III) mit verschiedenen Halogeniden, Pyridin und Methylpyrazin.
Authors: Scheffler A. , Preetz W.
Published: March 2015

The preparation of the mixed complexes mer-[OsBrnI3-n(Py)2(Mepyz)], n = 1, 2, by substituting or oxidizing exchange of the halide ligands and the chromatographic isolation of the pure compounds is described. Some steps of the successive substitution reactions take a stereospecific course due to the different trans-effects of I- and Br-.
Darstellung, Infrarotspektren und Strukturen einiger dimerer und polymerer Oxochloro- und Oxooxalato-isothiocyanato-Komplexe des Molybdän(V).
Authors: Mattes Rainer , Altmeppen Dirk , Fetzer Manfred
Published: March 2015

The crystal structure of (PyH)2(Mo2O4Cl4) · 3 H2O, earlier formulated as tetrameric di-μ-oxo-bis(di-µ-oxo-oxotetrachloroaquodimolybdate(V)), [(PyH)4][Mo4O8Cl8(H2O)2], has been determined. The structure consists of the dimeric anions [Mo2O4Cl4]2- with strong Mo=O ••• Mo interactions along the short c axes (c = 4.11 Å). The polymeric

[N(CH3)4]2[Mo2O3(C2O4)(NCS)4] and the dimeric [(PyH)4][Mo2O3(C2O4)2(NCS)4]

have been synthetized and characterized by infrared spectra and magnetic properties.
Reactions with 5,6,7-Trihydro-5,7-diarylthiazolo [3,2-b] -s-triazin-3(2 H)-ones
Authors: Abdel-Wahid Soliman Adly
Published: March 2015

4,6-Diaryl-2-carboxymethylthio-3,4,5,6-tetrahydro-s-triazines are cyclised to 5,6,7-trihydro-5,7-diarylthiazolo[3,2-b]-s-triazine-3(2H)-ones (3). 2-Arylmethylene-5,6,7-trihydro-5,7-diarylthiazolo[3,2-b]-s-triazin-3(2H)-ones (4) were prepared by several methods. Compounds 3 coupled with diazotised anilines to give 2,3,5,6,7-pentahydro-5,7-diarylthiazolo[3,2-b]-s-triazine-2,3-dione 2-arylhydrazones (5). The action of amines on 3 a opens the thiazolone ring with the formation of substituted (4,6-diphenyl-tetrahydrotriazin-2-ylthio)-acetamides (6).
Synthesen von Heterocyclen, 198 Zur Chemie der vicinalen Triketone, VII. Chinolino-benzoxazine und Chinolino-benzoxazepine aus 2.3.4-Trioxo-1.2.3.4-tetrahydro-chinolinen.
Authors: Wittmann Helga , Herzog Reinhard
Published: March 2015

2,3,4-Trioxo-l-phenyl-1,2,3,4-tetrahydro-quinoline (Ph—CHi) and 1,2,3-Trioxo-2,3,6,7-tetrahydro-1 H,5 H-benzo [ij] quinolizine (TMCHi) react with primary arylamines via “semiaminales” of type 1 to give quinolino-benzoxazinones of type 2 in high yields. Quinolino-benzoxazepines of type 3 are obtained with 2,6-dimethylaniline. However the N-unsubstituted 2,3,4-trioxo-1,2,3,4-tetrahydroquinoline (CHi) reacts under similar conditions only with 2-chloro- or 2,6-dimethyl-aniline to yield the corresponding ringclosed products 2 b and 3 a.
Synthesen von Heterocyclen, 199. Zur Chemie der vicinalen Triketone, VIII. Spiro-lactone aus 1.2.3-Trioxo-2.3-dihydro-phenalen sowie 2.3.4-Trioxo-1.2.3.4-tetrahydrochinolinen und Anthranilsäure.
Authors: Wittmann Helga , Taleban Hossein , Herzog Reinhard
Published: March 2015

1,2,3-Trioxo-2,3-dihydro-phenalene (PT) and 1,2,3-trioxo-2,3,6,7-tetrahydro- 1 H, 5 H-benzo[ij]quinolizine (TMCHi) react with anthranilic acid (AS) primarily to give the spirolactones 1 a-1 b, which are thermically rearranged to the corresponding benzoxazine carboxylic acids 2 a-2 b. 1-phenyl-2,3,4-trioxo-1,2,3,4-tetrahydro-quinoline (PHCHi) reacts with AS yielding the spirolactone 1 c, which decomposes upon heating.
Notizen: Preparation and Crystal Structure of the Hydrogen-Bonded Cyclic Dimer of PhP(S)[N(CH2Ph)2]OH, HN(CH2Ph)2+
Authors: Cameron T. Stanley , Healy James D. , Shaw Robert A. , Woods Michael
Published: March 2015

The structure of the title compound was determined by X-ray crystallography. The compound is a cyclic dimer with short N···O and N···S contacts.
Notizen: Gezielte Synthese von Sulfinato-O̲- und -S̲-Komplexen einiger Übergangsmetalle, XVI1 Sulfinato-S̲-Komplexe von Palladium(II) mit schwachen Donorliganden.
Authors: Lorenz Ingo-Peter , Lindner Ekkehard , Reuther Wolfgang
Published: March 2015

The complexes Na[(RS(O)2)2PdClL] (L = CH3CN (2), (CH3)2CO (3), THF (4)), stable in solid state, are obtained by substitution of H2O by weak donor ligands from Na[(RS(O)2)2PdCl(OH2)] (1). Their special reactivity in solution is shown by the ready substitution of all ligands, RSO2⁻ included. The IR spectra are discussed.
Bis[cyclotri(phosphazen)yl] oxide. / Bis[cyclotri(phosphazen)yl]oxides
Authors: Schmidpeter Alfred , Blanck Klaus , Högel Johann
Published: March 2015

Hydrido-cyclotri(phosphazen)es can be coupled by one or two step oxidation to give symmetric and unsymmetric bis[cyclotri(phosphazen)yl]oxides. Their structure follows from the analysis of their NMR spectra
Synthesen von Heterocyclen, CC Reaktionen mit cyclischen Oxalylverbindungen, XVIII Zur Reaktion von 4-Benzoyl-5-phenyl-2,3-dihydrofuran-2,3-dion mit Η-aktiven Nucleophilen. / Syntheses of Heterocycles, CC Reactions of Cyclic Oxalyl Compounds, XVIII The Reaction of 4-Benzoyl-5-phenyl-2,3-dihydrofuran-2,3-dione with Η-active Nucleophiles
Authors: Kollenz Gert , Ziegler Erich , Ott Walter , Igel Herwig
Published: March 2015

Hydrolysis of 4-Benzoyl-5-phenyl-2,3-dihydrofuran-2,3-dione (1) in water (ethanol) gives dibenzoylmethane and oxalic acid (ethyl ester). 1 reacts with aniline or p-toluidine yielding the 2-pyrrolones (2), which on the other hand are synthesized by addition of the corresponding anilines to the pyrrol-2,3-diones (8). 3 a adds methanol to give the 2-pyrrolone (4), which with aniline can be converted into 2 a. 2 a, b show fragmentation to oxalic acid anilides by heating (2 b) or treating with diazomethane (2 a). The reaction of 1 with p-nitroaniline leads via the furanone-derivative 6 to oxalic acid-di-p-nitroanilide. 1 and N-methylaniline combine to acrylic acid-N-methylanilide (7), which by heating gives the dibenzoyl acetic acid-N-methylanilide
Notizen: Ternäre Verbindungen in den Dreistoffsystemen Lithium(Natrium)-Beryllium-Arsen. / Ternary Compounds in the System Lithium(Sodium)-Beryllium-Arsenic
Authors: Schuster Hans-Uwe , Tiburtius Christoph
Published: March 2015

By investigations in the system

Li(Na)-Be-As

we found two new phases of the formula LiBeAs and NaBeAs which crystallize in a tetragonal resp. hexagonal structure
Notizen: Neutronenbeugungsuntersuchungen an den Phasen LiAlSi und LiAlGe. / Investigations on Neutron Diffraction of the Phases LiAlSi and LiAlGe
Authors: Schuster Hans-Uwe , Hinterkeuser Heinz-Walter , Schäfer Wolfgang , Will Georg
Published: March 2015

By neutron diffraction we found a decision on the distribution of the Al-Si(Ge)-atoms and the location of the lithium-atoms in the structures of the compounds LiAlSi and LiAlGe
Photoelektronenspektren und Moleküleigenschaften, LXIV. Dimethyldiselenid — ein Beispiel für die Wechselwirkung zwischen benachbarten Elektronenpaaren / Photoelectron Spectra and Molecular Properties, LXIV. Dimethyldiselenide - an Example for the Interaction between Adjacent Electron Pairs
Authors: Tschmutowa Galina , Bock Hans
Published: March 2015

The well-resolved helium(I) photoelectron spectrum of H3C-Se—Se-CH3 exhibits distinct bands corresponding to 11 of the total 13 valence electron ionizations. The unequivocal assignment is supported by EHMO calculations including spin/orbit coupling. The two selenium lone pair ionizations differ by 0.23 eV; a split observed also for dimethyl disulfide and discussed within a general model for interactions between adjacent lone pairs.
Totalsynthese von Somatostatin, I / Total Synthesis of Somatostatin, I
Authors: Kalbacher Hubert , Bürvenich Claus , Fuchs Stefan , Horn Hans , Klingler Wolfgang , Pietrzik Emanuel , Zech Karl , Voelter Wolfgang
Published: March 2015

Experimental details of the syntheses of five peptide fragments, used for the total synthesis of somatostatin, are described. N-Hydroxysuccinimide esters and DCC are used for forming the peptide bonds. The amino acid side chains are protected by trityl, tertbutyloxycarbonyl and benzyl groups.
Notizen: The 13C NMR Spectra of Organotransition Metal Complexes, I.
Authors: Hoffmann E. G. , Jolly P. W. , Küsters A. , Mynott R. , Wilke G.
Published: March 2015

The 13C NMR spectra of a number of nickel complexes of 1,5,9-cyclododecatriene and bicyclo-[2,2,1]-heptene have been studied and it has been shown that detailed structural information can be obtained relatively easily.
Notizen: Synthesen von Heterocyclen, 202. Mitt. Zur Chemie der vicinalen Triketone, IX / Syntheses of Heterocycles, 202. The Chemistry of Vicinal Triketones, IX
Authors: Wittmann Helga , Ehrlich Ernst , Siegel Hannes , Sterk Heinz
Published: March 2015

The reaction product of N-phenylquinisatine and diazomethane - formulated by EISTERT and DONATH3b as benzazepine (1) - has the 2,4-dioxo-1-phenyl-1,2,3,4-tetrahydroquinoline-3-spiro-2′-oxirane (2) structure as shown by 13C NMR spectroscopy.
Notizen: Photochemistry of Selenol Esters
Authors: Martens Jürgen , Praefcke Klaus , Simon Helmut
Published: March 2015

Depending upon the structure of the starting compounds, seleno-photo-Fries products or cyclization products (phenenthrenequinone or selenoxanthone) are obtained in novel photoreactions from areneselenol esters of aromatic carboxylic acids.
Untersuchungen über die Existenz einer Verbindung aus Bortrifluorid und Stickstoffmonoxid / On the Existence of a Compound with Boron Trifluoride and Nitrogen Monoxide
Authors: Hoffmann Karl-Friedrich , Minkwitz Rolf
Published: March 2015

By investigating infrared spectra of solid BF3-NO- (and BF3-15NO-)mixtures it is suggested, that addition compounds are formed at low temperatures. The assignment of bands and possible structures are discussed.
Diin-Reaktion, 431 Synthese und komplexchemische Umsetzung von 1.2.4.5-Tetra(phenylpropinoyl)-benzol / Diin Reaction, 431 Synthesis and Complex-chemical Reaction of 1,2,4,5-Tetra(phenylpropynoyl)-benzene
Authors: Hambrecht Jürgen , Müller Eugen
Published: March 2015

The Grignard-addition of phenylethynylmagnesium bromide to 1,2,4,5-tetraformylbenzene (1) and the subsequent oxidation of the primary formed alcohol (2) afford the l,2,4,5-tetra(phenylpropynoyl)benzene (8). The reaction of 8 with tris(triphenylphosphin)-rhodium-(I)chloride leads to the Rh-complex (4), which further reacts with acetylenederivates and chalcogens to form the quinoid compounds 5a-c and 6, 7.
Hydration of endo-Tricyclo[5,2,1,02,6]deca-3,8-diene (endo-Dicyclopentadiene) / Über die Hydratisierung von endo-Tricyclo[5.2.1.02,6]deca-3.8-dien (endo-Dicyclopentadien)
Authors: Roth K.
Published: March 2015

The hydration of endo-dicyclopentadiene (1) yields a 1:2 mixture of exo-8-hydroxy-exotricyclo[5,2,1,02,6]dec-3-ene (2) and exo-9-hydroxy-exo-tricyclo[5,2,1,02,6]dec-3-ene (3). The structures of these compounds were determined by 1H and 13C spectroscopy with simultaneous application of paramagnetic shift reagent Eu(fod)3. The stereospecific exoattack of the proton in the first reaction step is demonstrated by the reaction in deuteriumoxid.
Die Molekül- und Kristallstruktur von 1-Methyl-bis(dichlorphosphazo)-sulfonimid, N3P2SO2Cl4CH3, einer Verbindung mit der endocyclischen Gruppierung N3P2S / The Crystal and Molecular Structure of 1-Methyl-bis(dichlorophosphazo)-sulphonimide, N3P2SO2Cl4CH3, a Species with the Endocyclic Group N3P2S
Authors: Nuber Bernhard , Ziegler Manfred L.
Published: March 2015

The structure of N3P2SO2Cl4CH3 was determined from three-dimensional X-ray data by direct sign determination. The heterocyclic compound with the endocyclic group N3P2S has a chair conformation.
Über die Darstellung linearer Thiazene / Preparation of Linear Thiazenes
Authors: Steinbeisser Hartmut , Mews Rüdiger , Glemser Oskar
Published: March 2015

(CF3)2CNSCl (1) and amines, silylated amines, and silver salts react to form linear thiazenes and carbothiazenes e.g. [(CF3)2C=N-S-]3N (5), (CF3)2C=N-S-N = SF2 (6), (CF3)2C=N-S-N=S=N-SiR3 (7), (CF3)2C=N-S-NCO (8), and [xxx] (9).
29Si-Kernresonanzuntersuchungen an N-Trimethylsilyl-substituierten Aminen und Amiden / 29Si Nuclear Magnetic Resonance Studies on N-Trimethylsilyl Derivatives of Amines and Amides
Authors: Heinz B. , Marsmann H. C. , Niemann U.
Published: March 2015

The 29Si chemical shifts of several trimethyl silyl derivatives of amines and amides are measured and compared to other chemical and theoretical properties such as the basicities or the electronic charge on the nitrogen or the hydrogen of the N-H group of the amine or the amide. Whereas the 29Si chemical shift of saturated amines can be rationalized in terms of substituent effects, the shifts of aromatic amines show some dependency on the basic character of the amine. There seems to be little correlation between 29Si chemical shifts and electronic charge, but there is a similarity of 29Si with 1H chemical shifts of the NH group, which is interpreted as depending on anisotropy effects.
Reaktionen von 1.4-Dienen mit Metallkomplexen, II. Darstellung und Röntgenstrukturanalyse von Chloro-(η3-1-methylen-3-methylcyclohexyl)(triphenylphosphin)palladium(II), (C8H13)PdClP(C6H5)3 / Reaction of 1,4-Dienes with Metal Complexes, II. Synthesis and X-ray Structure Determination of (η3-1-methylene-3-methylcyclohexyl)(triphenylphosphine)palladium(II), (C8H13)PdClP(C6H5)3
Authors: Zeiner Hartmut , Ratka Richard , Ziegler Manfred L.
Published: March 2015

The compound (C8H13)PdClP(C6H5)3 has been synthesized and its structure determined from three-dimensional X-ray data.
Photolysis (A = 185 nm) of Liquid Acetaldehyde Dimethyl Acetal
Authors: Schuchmann Heinz-Peter , Von Sonntag Clemens
Published: March 2015

Deaerated liquid acetaldehyde dimethyl acetal has been photolyzed at λ = 185 nm, and 28 products have been determined. The major ones with their quantum yields are: methanol (0.59), methane (0.26), ethyl methyl ether (0.17), methyl vinyl ether (0.16), methyl formate (0.14), ketene dimethyl acetal (0.1), ethane (0.06), hydrogen (0.06), and acetaldehyde (0.06).

The major primary processes are suggested to be the scission of the C-OCH3 bonds (homolytic and molecular) and of the O-CH3 bonds (homolytic). Minor processes are hydrogen elimination reactions and the scission of the C-CH3 bond.
Zur Synthese von phosphorhaltigen Heterocyclen mit metallorganischen Verbindungen / Synthesis of Phosphorus Containing Heterocycles with Metal Organic Compounds
Authors: Roesky Herbert W. , Zamankhan Hamid
Published: March 2015

CH3P(S)(NCO)2 reacts with [(CH3)3Si]2N-CH3, [(CH3)3SiNCH3]2CO and [(CH3)3Sn]3N to give the cyclic compounds 2a-2c. The structures are discussed on the basis of NMR and IR data. In 2 a and 2 b the (CH3)3Si-groups are easily and quantitatively replaced by protons with water under formation of (CH3)3Si-O-Si(CH3)3. By the reaction of CH3P(S)(NCO)2 with [(CH3)3Si]2S 4 is obtained, a cyclic compound with a sulfur atom of coordination number 2.

FP(S)(NCS)2 was used to investigate the scope of these reactions. With [(CH3)3Si]2NCH3 and FP(S)(NCS)2 5 is obtained, which reacts with S2Cl2 to yield 6, a bridged disulfur compound. This method may be useful for the systematic investigation of new cyclic compounds.
15N-NMR-Untersuchungen an Verbindungen mit direkten N-N-Bindungen / 15N NMR Studies on Compounds with Direct N-N Bonds
Authors: Schultheiss Harald , Fluck Ekkehard
Published: March 2015

15N chemical shifts, the isotopic effect on chemical shifts and 1J(15N-15N) coupling constants of Na2N2O3, K2SO3N2O2, Na2[CH2(N2O2)2], [(C2H5)2NH2][(C2H5)2NN2O2] and N2O3 were measured. The discussion is based on a compilation of reported 15N-15N coupling constants.
Reactions with o-Phenylenediamine Preparation of 2-Substituted Benzimidazoles and Benzimidazole-ethylenes
Authors: Hammad M. , Emran A.
Published: March 2015

o-Phenylenediamine reacts with arylidenecyanoacetic acid derivatives and with analogous arylmethylidenemalononitriles to give 2-arylbenzimidazoles (6). 2-Cyanomethylbenzimidazole (7) reacts with aromatic aldehydes to give 1-aryl-2-cyano-2(2-benzimidazole)ethylenes (8). The reduction products of the latter compounds are, also, presented. Structures of the newly prepared compounds have been proved using micro and spectral analyses.
Preparation of Spin-Labeled Phosphoroamidates in High Yield Using Imidazole as the Transfer Agent
Authors: Sosnovsky G. , Konieczny M.
Published: March 2015

The spin-labeled (1-oxyl-2,2,6,6-tetramethyl-4-piperidyl)-phenyl imidazole-1-phosphonate (4) was used to prepare (1-oxyl-2,2,6,6-tetramethyl-4-piperidyl)phenyl N-alkyl and N-aryl phosphoroamidates (8) in yields generally exceeding 70%.

[xxx]

Amidates 8 were also prepared from the corresponding chloridate 10. However, in the latter case, a basic condensing agent, such as, triethylamine was essential. The chloridate 10 was converted to the spin-labeled pyrophosphate 11 and the acid 12.

[xxx]

The pyrophosphate 11 can be employed to phosphorylatively spin-label amines.
Notizen: AB2X2-Verbindungen im CaAl2Si2-Typ, II1 (A = Ca; B = Zn, Cd; X = P, As) / AB2X2 Compounds with the CaAl2Si2 Structure, II1 (A = Ca; B = Zn, Cd; X = P, As)
Authors: Klüfers Peter , Mewis Albrecht
Published: March 2015

Four new ternary calcium compounds of zinc (cadmium) with a 5B-element have been prepared. Analytic, pycnometric and X-ray powder data are given. The compounds are supposed to crystallize trigonally in a CaAl2Si2-type structure.
Notizen: Darstellung und Struktur der Phase Li2Sb / Preparation and Crystal Structure of Li2Sb
Authors: Müller Wiking
Published: March 2015

The new intermetallic compound Li2Sb has been prepared and its crystal structure has been determined. It crystallizes hexagonally, a = 794.6 ± 0.5 pm, c = 652.7 ± 1.0 pm, c/a = 0.821, space group P 6̅2c–D3h
4 isotypic with Mg2Ga. Relations to the Zintl-phases are discussed.
Darstellung und Kristallstruktur von BaMnSb2, SrMnBi2 und BaMnBi2 / Preparation and Crystal Structure of BaMnSb2, SrMnBi2 and BaMnBi2
Authors: Cordier Gerhard , Schäfer Herbert
Published: March 2015

BaMnSb2, SrMnBi2 and BaMnBi2 have been prepared and structurally characterized. The new compounds are isotypic and crystallize tetragonal in the SrZnBi2 structure with the following constants:

BaMnSb2: a = 4.53 ± 0.01 Å, c = 24.34 ± 0.03 Å, c/a = 5.37.

SrMnBi2: a = 4.58 ± 0.01 Å, c = 23.13 ± 0.03 Å, c/a = 5.05.

BaMnBi2: a = 4.63 ± 0.02 Å, c = 24.22 ± 0.05 Å, c/a = 5.23.

The transition metal atoms form together with the semimetal atoms sheets of tetragonal pyramids separated by double layers of alkali earth atoms. In these double layers there are inserted Bi/Sb-square nets.
Darstellung von Heteropolymolybdaten in organischen Lösungsmitteln / Preparation of Heteropolymolybdates in Organic Solvents
Authors: Fuchs Joachim , Brüdgam Irene
Published: March 2015

Heteropolymolybdates are obtainable from nonaqueous solutions. They are formed by reaction of molybdates or isopolymolybdates soluble in organic solvents with oxo acids or metal salts.

Compounds with the anions TeMo6O24
6-, MIIIMo6O24H6
3- (MIII = Fe, Al, Cr), ΜIIMo6O24Η6
4- (MII = Zn, Cu, Co, Ni), PMo12O40
3-, as well as the novel heteropolyanion Ρ2Mo4O19
4- were obtained.

The IR and Raman spectra are discussed.
Study of the Reactivity of 2-Cinnamoylbenzimidazole towards Thiourea, Urea, Hydrazines and Hydroxylamine Hydrochloride
Authors: Zoorob H. H. , Hammouda H. A. , Ismail E.
Published: March 2015

The reactivity of heterocyclic α,β-unsaturated ketones towards the title compounds has been studied. A pyrimidine, pyrazoline, isoxazoline and a fused pyrrolidine rings have been built up. Mannich reaction was tried with the pyrazoline derivative (4 d). Bromination of the 2-cinnamoyl compounds (1 a-c), and cyclization of the products were also undertaken.
Complex of Diphenylcyclopropenone with Substituted Acetic Acid and Formic Acid
Authors: Sridhara Narendra S. , Singh Rajendra
Published: March 2015

Reaction of diphenylcyclopropenone with bromoacetic acid, trifluoroacetic acid and benzoylformic acid leads to crystalline complexes.
Notizen: Reaktion von Natriumanilid mit Natrium-Pentacyanonitrosylferrat(II) / Reaction of Sodium Anilide with Sodium Pentacyanonitrosylferrate(II)
Authors: Nast Reinhard , Schmidt Jörn
Published: March 2015

Na2[Fe(CN)5NO] reacts with two molar equivalents of sodium anilide in liquid ammonia forming a yellow crystalline diamagnetic complex Na4[Fe(CN)5N(O)NC6H5]. The reaction is an analogon to the well-known nucleophilic attack of OH- ions in water which yields pentacyanonitroferrate (II).
Notizen: Darstellung des Benzolmangantricarbonyl-Kations aus Methylcyclopentadienylmangantricarbonyl / Preparation of Cationic Benzene-manganese-tricarbonyl from Methylcyclopentadienyl-manganese-tricarbonyl
Authors: Bachmann Paul , Repp Karl-Rudolf , Singer Hellmut
Published: March 2015

Exchange of the cyclopentadienyl ligand from methylcyclopentadienyl-manganese-tricarbonyl by benzene, toluene, xylene, mesitylene and other aromatics with AlBr3 as catalyst gives cationic aromatic manganesetricarbonyl complexes. The amount of AlBr3 and the addition of aqueous HBr do not only influence the yield but also the purity of the products. With this new method

C6H6Mn(CO)3+

can be prepared in high yield from a relatively inexpensive starting material.
1H-, 13C-, 29Si-NMR. und 35,37Cl-NQR-Spektren von (Chlormethyl)silan, H3SiCH2Q / 1H, 13C, 29Si NMR and 35
.37Cl NQR Spectra of (Chloromethyl)silane, H3SiCH2Cl
Authors: Schmidbaur Hubert , Zimmer Beate , Köhler F. H. , Buchner Wolfgang
Published: March 2015

1H,13C, 29Si NMR and 35,37Cl NQR spectra have been obtained for (chloromethyl)silane, H3SiCH2Cl. The results are compared with the corresponding parameters of ethyl chloride, H3CCH2Cl. A less polar C—Cl bond is found in the silicon compound, due to the electronic effect of the silyl group H3Si. Previous findings are in agreement with this conclusion.
Ein Beitrag zur Kristallchemie dreiwertiger Seltenerdoxide Zur Stabilisierung der monoklinen B-Form / About the Crystal Chemistry of Three-Valent Rare Earth Oxides The Stabilisation of the Monoclinic B-Modification
Authors: Muschick W. , Müller-Buschbaum Hk.
Published: March 2015

Single crystals of 1—x Ho2O3 : xCaO (x = 0.07), CaHoO2.5 (A) and Ca0.5Ho1.5O2.75 (B) were prepared by high temperature reaction and investigated with X-ray single crystal data. It can be shown that small amounts of CaO stabilize the monoclinic B-Typ of rare earth oxides. Phase (A) and (B) cannot be seen as a stabilized B-type crystal because they have an new crystal structure with space group

C2
2h–P 21/m, a = 656.6, b = 356.7, c = 529.4 pm, β = 92.3°; a = 650.2, b = 352.4, c = 584.5, β = 92.3°.
Reaktionen von Halogeno-Phosphin-Metall(II)-Komplexen mit organischen Aziden. Phosphatriazen-Kobalt(II) -Komplexe / Reactions of Halogeno Phosphine Metal(II) Complexes with Organic Azides. Phosphatriazene Cobalt(II) Complexes
Authors: Beck Wolfgang , Rieber Wolfram , Kirmaier Helmut
Published: March 2015

The phosphine complexes Co(PR3)2X2 (X = Cl, Br; R = Et, Ph, C6H11) react with furoylazide (furN3) at 25 °C to give the phosphinimine compounds Co(furN=PR3)2X2. At lower temperatures the intermediate complex Co[furN3P(C6H11)3]Br2 • Et2O with phosphatriazene as ligand could be isolated.
Die Komplexbildung von Tris(dihydroxy-phosphonylmethyl)phosphinoxid* mit einigen zweiwertigen Kationen / Complex Formation of Some Divalent Cations with Tris(dihydroxy-phosphonylmethyl)phosphine Oxide
Authors: Anderegg G.
Published: March 2015

The formation of the 1:1 complexes of Mg2+, Ca2+, Ni2+, Cu2+ and Zn2+ with tris-(dihydroxy-phosphonylmethyl)phosphine oxide has been studied by pH measurements. The values of the stability constants and their trend is similar to that found for the complexes of tripolyphosphate.
Condensed 1,2,4-Triazines, II Synthesis and Structure of Some Phenanthro [9,10-e] -1,2,4-triazolo [4,5-b] -as-triazine Derivatives
Authors: Ibrahim Y. A. , Zaher H. A. , Abdel-Hady S. A. L.
Published: March 2015

3-Hydrazinophenanthro[9,10-e]-1,2,4-triazine (2) was prepared and condensed with aromatic aldehydes to give the corresponding arylidene derivatives (3 a–f). Phenanthro-[9,10-e]-1,2,4-triazolo[4,5-b]-as-triazine (11), its 3-mercapto- (4 a), 3-alkylmercapto- (9 a–d) and 3-hydroxy- (4b) derivatives were prepared and their structures have been established.
Notizen: Homogene katalytische Hydrierung ungesättigter Carbonsäureester mit H2PtCl6 + SnCl2 in iso-Butanol / Homogeneous Catalytic Hydrogenation of Unsaturated Carboxylic Acid Esters with H2PtCl6 + SnCl2 in iso-Butanol
Authors: Strohmeier Walter , Weigelt Luise
Published: March 2015

The catalytical system, prepared from H2PtCl6 + SnCl2 · 2 H2O and the additives HBr and H2O in iso-butanol is very efficient for homogeneous hydrogenation of unsaturated esters under mild conditions. Reaction rates r up to 40 mMol · 1-1 · min-1 and turnover numbers UZ higher than 1.600 are observed.
Notizen: Phosphoranes with a Chiral Centre Containing the 1,2-Oxaphosphetane Ring System
Authors: Gibson James Andrew , Röschenthaler Gerd-Volker , Schmutzler Reinhard
Published: March 2015

Hexafluoroacetone and tetramethyldiphosphine react readily at low temperatures producing three 4,4-bis(trifluoromethyl)-1,2-oxaphosphetanes (1), (2), and (3). The compounds have chiral centres at phosphorus producing doubling of resonances in the NMR spectra.
Notizen: Tellurium Heterocycles, I Synthesis of 2,3-Dihydrotellurolo(2,3-b)quinolines
Authors: Ramasamy K. , Shanmugam P.
Published: March 2015

The literature is replete with reports on furo-1,2 and thieno-(2,3-b)quinoline2 syntheses. But hitherto, there is only one report on the selenium3 and no report on the tellurium analogs. In connection with our work1,2 on furo(2,3-b)quinolines, we prepared several 3-(2′-hydroxyethyl)-2-quinolones and we felt that it might be possible to transform them, by an appropriate sequence, into the corresponding selenolo- and tellurolo-(2,3-b)-quinolines. Recently we have reported3 the synthesis of several 2,3-dihydroselenolo-(2,3-b)quinolines, achieved through the use of 2-chloro-3-(2′-chloroethyl)quinolines, obtained from the corresponding 3-(2′-hydroxyethyl)-2-quinolones by POCl3-treatment. Simultaneously we were exploring the feasibility of obtaining the tellurium analogs in a similar fashion.
Organische Schwefelverbindungen, XXIV1,2 Kettenlängen-Effekte bei massenspektrometrischen Zerfällen von α,ω-Dithiodicarbonsäure-S.S′-di-p-tolylestern / Organosulfur Compounds, XXIV1,2 Chain Length Effects in Mass Spectroscopic Decompositions of S,S′ -di-p-tolyl-α,ω-bis(thioates)
Authors: Martens Jürgen , Praefcke Klaus , Schulze Ursula , Schwarz Helmut , Simon Helmut
Published: March 2015

The study on the mass spectroscopic behavior of the title compounds is based on AP-measurements, the investigation of deuterated derivatives, and the analysis of chain length effects. It is shown that, among other things, the stable [M-STol]+-ions produced by 9 homologs will not enter a cyclization reaction within 10-5 sec. The reactive [M-STol]+-species of S,S′-di-p-tolyl dithioadipate possess an abnormal fragmentation behavior (consecutive lass of CO and H2O), the details of which are elucidated by employment of 2H-labelled compounds and investigation of S,S′-di-p-tolyl 2,5-dimethyldithioadipate. Obviously, the sulfur of the thiol ester group seems to play a decisive role in this and other decomposition processes.
On the Formation of Alkenylaryl Nitroxide Free Radicals in the Photolysis of 2-Nitrobenzaldehyde-olefin Systems
Authors: Filby W. G. , Günther K.
Published: March 2015

The origin and nature of the radicals arising during the photolysis of 2-nitrobenzaldehyde in the presence of olefin quenchers is discussed. The radicals, assigned an alkenylaryl nitroxide structure, arise via a dark Diels-Alder reaction involving product nitroso benzoic acid and the olefine.