Synthesen des 4-Sulfanilamido-5,6-dimethoxypyrimidins

Zusammenfassung Es wird über 4 verschiedene Synthesen des 4-Sulfanilamido-5,6-dimethoxypyrimidins² berichtet.Frau Prof. Dr. Dr.E. Cremer zum Geburtstage in Verehrung gewidmet.14. Mitt.:H. Bretschneider, J. Dehler undW. Klötzer, Mh. Chem.95, 207 (1964).     

Eu3+ und Eu2+ in Oxometallaten der Zusammensetzung MBeLn2O5: SrBeEu2O5 und EuBeNd2O5

Eu³⁺ and Eu²⁺ in Oxides of the Composition MBeLn₂O₅: SrBeEu₂O₅ and EuBeNd₂O₅ Single crystals of (I): SrBeEu₂O₅ and (II): EuBeNd₂O₅ were prepared by CO₂-LASER (I) in air and plasma torch (II) technique in H₂ atmosphere. X-ray investigations led to orthorhombic symmetry, space group D-Pnma; (I): a = 9.488, b = 7.156, c = 6.495 Å; (II): a = 9.534, b = 7.225, c = 6.544 Å, Z = 4. Sr²⁺ and Eu³⁺ as well as Eu²⁺ and Nd³⁺ are in statistical distribution within a Kagomé framework. Both compounds are discussed with respect to the monoclinic form of MBeLn₂O₅.     

Darstellung und Kristallstruktur der isotypen Verbindungen Ca2Os3B5 und Eu2Os3B5

Preparation and Crystal Structure of the Isotypic Compounds Ca₂Os₃B₅ and Eu₂Os₃B₅ The isotypic borides Ca₂Os₃B₅ and Eu₂Os₃B₅ crystallizing in the monoclinic space group C2 with Z = 2 were prepared by reaction of the elemental components in sealed tantalum tubes (lattice constants see Inhaltsübersicht). The structure contains puckered osmium-boron layers connected by boron atoms with very short Os? B distances.     

Schwingungsspektroskopische Untersuchungen an As2O5 und AsSbO5

Vibrational Spectroscopic Investigations on As₂O₅ and AsSbO₅ Raman, IR and FIR spectra of As₂O₅ and of the isostructural AsSbO₅ in the range of 30 to 1000 cm^?1 are reported. On the basis of factorgroup analysis and of the information, provided by the exchange of 6-fold coordinated arsenic for antimony, several bands can be assigned.     

Zweiwertiges Neodym: NdCl2 und KNd2Cl5

Divalent Neodymium: NdCl₂ and KNd₂Cl₅ Single crystals of NdCl₂ have been obtained via metallothermic reduction of NdCl₃ with lithium: a = 908.49(5), b = 761.47(5), c = 455.62(2) pm, Pbnm, Z = 4, PbCl₂ type, refined to R = 0.047. Reduction of NdCl₃ with potassium yields KNd₂Cl₅: a = 894.51(9), b = 785.16(7), c = 1 265.28(13) pm, β = 90.000(8)°, P2₁/c, Z = 4, isotypic with TlPb₂Cl₅. There is a close structural relationship of KNd₂Cl₅ with K₂NdCl₅.     

Darstellung und Reaktionen von 5-Amino-2H-imidazolen

Zusammenfassung 2,4,5-substituierte 5-Amino-2H-imidazole entstehen mit guten Ausbeuten durch Behandlung einer Lösung der entsprechenden Imidazolin-³-thione-(5) in Äthylenglykol mit NH₃ bei 80°.Die Reaktionsfähigkeit der neuen Verbindungen wird am Beispiel des 2-Methyl-2,4-diphenyl-5-amino-2H-imidazols untersucht. Bei der Acetylierung, Benzoylierung sowie der Umsetzung mit Benzolsulfochlorid, Phenylisocyanat und Phenylsenföl reagiert die exocyclische Aminogruppe; die Alkylierung mit CH₃J erfolgt dagegen am Ringstickstoff. Die Umsetzung mit Acetessigester oder Malonsäurediäthylester führt zum neuen bicyclischen System der 5H-Imidazo[1,5-a]pyrimidinone. Durch Reduktion mit NaBH₄-AlCl₃ entsteht mit geringer Ausbeute das entsprechende 5-Amino-imidazolidin.

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2,4,5-substituted 5-amino-2H-imidazoles are formed in good yields, when a solution of the corresponding ³-imidazoline-5-thione in ethylene glycol is treated with NH₃ at 80°.The reactivity of this new class of compounds has been investigated using 2-methyl-2,4-diphenyl-5-amino-2H-imidazole. On acetylation, benzoylation and in the reaction with benzenesulfonyl chloride, phenyl isocyanate and phenyl isothiocyanate, the exocyclic amino group reacts; alkylation with CH₃J, however, takes place at the ring nitrogen atom. The reaction with ethyl acetoacetate or ethyl malonate leads to the new bicyclic ring system of 5H-imidazo-[1,5-a]-pyrimidinones. Reduction with NaBH₄-AlCl₃ gives in lower yields the corresponding 5-amino-imidazolidine.

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45. Mitt.:F. Asinger, W. Schäfer undG. Kriebel, Mh. Chem.96, 69 (1965).

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Teil der Dissertation vonA. V. Grenacher, Techn. Hochschule Aachen. 1964.     

Darstellung und Kristallstruktur von NaBi2AuO5

Synthesis and Crystal Structure of NaBi₂AuO₅ NaBi₂AuO₅ was obtained by hydrothermal reaction of ‘Bi₂O₅’, Au₂O₃ · 2H₂O and saturated aqueous NaOH solution at temperatures from 300 to 600°C and oxygen pressure from 3 × 10⁸ to 6 × 10⁸ Pa for the first time. The crystal structure (P4 b2; a = 1 220.02(6) pm; b = 386.68(3) pm; Z = 4; R_w = 0.022) consists of bisphenoidic distorted AuO₄ groups, which are stacked in c-direction. They are connected by square pyramidal BiO₅ units. Sodium is occupying holes within the Au/Bi/O framework thus formed.     

Synthese und Kristallstruktur von Sr3Ga2O5Cl2 und Sr3Fe1.18Al0.82O5Cl2

Solid state reactions, by using a flux, lead to the new compounds Sr₃Ga₂O₅Cl₂ (A) and Sr₃Fe_1.18Al_0.82O₅Cl₂ (B). By means of single crystal X-Ray determinations a monoclinic symmetry (space group C ₂ ² -P2₁, (A):a=9.569 (2) Å; (B):a=9.550 (2) Å,Z=4) was found. Both compounds are not isotypic to Sr₃Fe₂O₅Cl₂ but crystallize like Ba₃Fe₂O₅Cl₂.

     

Synthese und Reaktionen des 2-Phenyl-tetrazol-5-carbaldehyds

The title compound is obtained from 2-phenyl-5-chloromethyl-tetrazole byKröhnke reaction. It undergoes the typical aldehyde reactions. Characteristic differences in the behavior of isomeric N-substituted tetrazoles are explained.     

Darstellung und kristallographische Daten von K2Si2O5, KHSi2O5I und K2Si4O9

K₂Si₂O₅ KHSi₂O₅I und K₂Si₄O₉ have, been synthesized partly by annealing and partly by hydrothermal treatment of glasses of suitable chemical composition. From powder and single crystal x-ray diagrams the lattice dimensions have been determined (see: ?Inhaltsübersicht”?).     

Pseudobrookite mit weitgehend geordneter Metallverteilung: CoTi2O5, MgTi2O5 und FeTi2O5

(A), (B) and (C) were prepared by solid state reactions. Single crystals of quenched samples were examined by X-ray investigation. On the opposite of A₂TiO₅-pseudobrookite compounds (A), (B) and (C) crystallize with a high ordered metaldistribution on the point positions 4c and 8f.     

Das Verhalten von Oxin, 2-Methyl-oxin, 5-Nitroso-oxin und 2-Methyl-5-nitrosooxin

Ohne Zusammenfassung     

Ein Wechsel des Strukturtyps in den Oxiden BaCoGd2O5, BaCoDy2O5 und BaCoY2O5

A Change of Structure Type in the Oxides BaCoGd₂O₅, BaCoDy₂O₅, and BaCoY₂O₅ (I) BaCoGd₂O₅, (II) BaCoDy₂O₅, and (III) BaCoY₂O₅ were prepared for the first time and examined by single crystal work. (I) and (II) belong to the BaNiLn₂O₅-type. (I): a = 3.770; b = 5.860; c = 11.620 Å; Z = 2; (II): a = 3.755; b = 5.798; c = 11.514 Å; Z = 2; space group D–Immm. (III) crystallizes in the BaCuLn₂O₅-type, space group D–Pnma, a = 12.287; b = 5.713; c = 7.067 Å; Z = 4. The coordination of Co²⁺ changes from (I, II) to (III) from octahedral to tetragonal pyramidal.     

Neue PdxAly-Phasen und die Verbindung Pd5AII2

New Pd_xAl_y Phases and the Compound Pd₅AII₂ The new phases Pd_2.4-2.9Al, Pd_2.99-3.3Al, and Pd_3.8-4.15Al were prepared by synthesis from molten mixtures and subsequent annealing at 600°C, or by reaction in the presence of iodine at 600°C, and were identified by X-ray powder diagrams. In the iodine-containing systems, the same phases resulted from the relation between composition of the gas phase and the structure of the solid reaction component. The existence of Pd₅Al₃ was confirmed. The new compound Pd₅AlI₂, the crystal structure of which was determined from a single crystal X-ray analysis, has a tetragonal layer structure with a = 405.2 and c = 1955.9 pm, space group I4/mmm. Iodine layers alternate with ordered Pd/Al slabs. The compound is a metallic conductor with highly preferred conductivity parallel to the layers.     

Struktur und Eigenschaften von 5-epi-Flavoxanthin und 5-epi-Chrysanthemaxanthin

Structure and properties of 5-epi-flavoxanthin and 5-epi-chrysanthemaxanthin The absolute configurations of 5-epi-flavoxanthin ( 6 ) and 5-epi-chrysanthemaxanthin ( 7 ) prepared by acid catalysed rearrangement of semi-synthetic lutein epoxide 5 are shown to be (3S, 5S, 8R, 3′R, 6′R) and (3S, 5S, 8S, 3′R, 6′R), respectively. Contrary to published data [5] the relationship of the polyene chain and H₃(18) on the dihydrofurane ring is cis for the pair of stereoisomers having a Δδ = δ (H? C(7)) ? δ (H? C(8)) = 0,22 ppm and ³J ≡ 0. These conclusions are in full accord with the chiroptical data.     

Die Synthese des VF5 aus V2O5 und Fluor

Ohne Zusammenfassung