Synthese und Eigenschaften einiger Phenoxyarylsilane

Ohne Zusammenfassung     

Synthese und Eigenschaften einiger Iodtrisilane

The syntheses and properties of the iodotrisilanes (IH₂Si)₂SiH₂, (IH₂Si)₂SiHI, I₃SiSiI₂SiH₃, (I₃Si)₂SiH₂ and Si₃I₈ are reported. All trisilanes were synthesized from the appropriate phenyltrisilanes and hydrogen iodide, with the exception of I₅Si₃H₃, which was prepared by thermolysis of I₃SiSiH₃. The ²⁹ Si-chemical shifts and ²⁹Si²⁹Si-coupling constants are reported. ab]Die Synthesen und Eigenschaften der Iodtrisilane (IH₂Si)₂SiH₂, (IH₂Si)₂SiHI, I₃SiSiI₂SiH₃, (I₃Si)₂SiH₂ und Si₃I₈ werden beschrieben. Bis auf I₅Si₃H₃, das während der Thermolyse von I₃SiSiH₃, entstand, wurden alle Iodtrisilane aus den entsprechenden Phenyltrisilanen mit Iodwasserstoff hergestellt. Die ²⁹Si-Verschiebungen und ²⁹Si²⁹Si-Kopplungskonstanten werden mitgeteilt.     

Synthese und Konformation einiger Tetraoxaspirane

Summary The synthesis of three new constitutionally symmetrical tetraoxaspirans with two oxygen atoms in the 7-membered ring is described. The structure of the compounds was determined by chemical and spectral evidence. Some aspects of the conformation of the compounds were studied using UV/VIS. Hypochromism was observed in the case of3.

     

Schwingungsspektren und Synthese einiger Phenyl- undp-Tolyldisilane

Summary The infrared and Raman spectra ofPh ₃SiSiH₃,Ph ₃SiSiD₃,Ph ₂HSiSiHPh ₂,Ph ₂DSiSiDPh ₂,PhH₂SiSiH₂ Ph andPhD₂SiSiD₂ Ph are reported and assigned with the aid of a normal coordinate analysis (NCA). The syntheses and vibrational spectra of thep-tolyldisilanespTol ₃SiSiH₃, andpTolH₂SiSiH₂ pTol are described, too.

     

Acyl- und Alkylidenphosphane. XII [1]. Synthese und Eigenschaften des 2,2-Dimethylpropionylphosphans und einiger Derivate

Acyl and alkylidene phosphines. XII. Syntheses and properties of 2,2-dimethylpropionylphosphine and of some derivatives At ?25°C bis(trimethylsilyl)phosphine 1b and 2,2-dimethylpropionyl chloride form (2,2-dimethylpropionyl)trimethylsilylphosphine 2b . As this compound is thermally more stable than similar acyltrimethylsilylphosphines, it might be treated at ?55°C with methyllithium to form the correspondig lithium phosphide 2d ; after the addition of chlorotrimethylsilane [2,2-dimethyl-1-(trimethylsiloxy)propylidene]-trimethylsilylphosphine 3c is obtained. At +20°C 2b rearranges to the E and Z isomer of [2,2-dimethyl-1-(trimethylsiloxy)propylidene]phosphine 3b . The NMR data of E- 3b and Z- 3b differ mostly in the coupling constants. Kept in the diffuse daylight for several days 3b dimerizes to form 2,4-di(tert.butyl)-2,4-bis(trimethylsiloxy)-1,3-diphosphetane 10 . In solution 10 is unstable and decomposes again to a mixture of the E und Z isomer of 3b . Reacting 3b or 3c with alcoholes all trimethylsilyl groups are replaced by hydrogen atoms and unstable 2,2-dimethylpropionylphosphane 4b is formed. Lithium(2,2-dimethylpropionyl)phosphide 4d , synthesized at ?60°C from 4b and methyllithium, crystallizes with one molecule 1,2-dimethoxyethane per formula unit and is dimeric in benzene. As shown by the NMR data 4d has the structure of an alkylidene-phosphine with the lithium atom bound to oxygen. At ?50°C 4d and chlorotrimethylsilane react to form 3b .     

Synthese und Konformation einiger Azaspirane mit Alkyl-bzw. Aryl-Sulfonamid-Gruppen

Preferred conformations of some azaspiran systems substituted with large groups at the nitrogen atoms were established by UV absorption spectroscopy. These groups prohibit the inversion at nitrogen, as was deduced from the¹H NMR spectra.

     

Synthese und Eigenschaften einiger h?hergliedriger cyclischer Atheracetale

Ohne Zusammenfassung     

Synthese einiger n-Alkylcycloalkane und Bestimmung ihrer Dichten und Viskositäten

Zusammenfassung Es wird die Darstellung einiger n-Alkylcyclopropane,-cycloheptane und-cyclooctane beschrieben. Die Dichten und Viskositätswerte, jeweils im Temperaturbereich von 20–80^o werden angegeben.11. Mitt. der Reihe Konstitution und physikalische Eigenschaften.9. Mitt.:R. Riemschneider undJ. Sickfeld, Mh. Chem.93, 933 (1962).     

Synthese einiger Glucuronid-Metaboliten von Phenacetin und Phenetidin,Teil II

The anomeric configuration of the main metabolite of phenacetin, p-acetamido-phenyl β-D -glucopyranosido-uronic acid, was established by configurative correlation with a cyclohexyl β-D -glucopyranosido-uronic acid derivative. Furthermore, some anomeric D -gluco-pyranoside conjugates of 2-ethoxy-5-acetamido-phenol were synthesized and characterized using NMR.-spectroscopy and ORD./CD.     

Zur Synthese einiger Siliciumstickstoffverbindungen

The preparation of 1-dimethylamino-hexamethyldisilazane, tridecamethyltetrasilazane and hexadecamethylpentasilazane is described. All the compounds are colourless liquids.     

Synthese und spektroskopische Charakterisierung einiger Pentacarbonylwolfram(0)-Komplexe mit verschiedenen 1H-Phosphiren-Liganden,Kristallstrukturen von,und

Synthesis and Spectroscopic Characterization of some Pentacarbonyltungsten(0) Complexes with Various 1H-Phosphirene Ligands: Crystal Structures of , and The tungsten(0) complex 1 reacts upon heating with acetylene derivatives 2a–f in toluene to form benzonitrile and the complexes 4a–f ( 4a : R¹ ? Ph, R² ? H; 4b : R¹ ? Ph, R² ? CH₃; 4c : R¹ ? OEt, R² ? H; 4d : R¹ ? Ph, R² ? CO₂Et; 4e : R¹, R² ? CO₂Me; 4f : R¹, R² ? SiMe₃), which have been isolated by chromatography. Spectroscopic and mass spectrometric data are discussed. The crystal structures of the compounds 4a, b and d were determined by X-ray single crystal structure analysis ( 4a : space group P2₁/n, Z = 4, a = 937,5(2) pm, b = 2202,4(6) pm, c = 1266,3(4) pm, β = 108,94(4)°; 4b : space group P2₁/c, Z = 4, a = 1293,9(2) pm, b = 923,5(1) pm, c = 2223,4(3) pm, β = 92,385(6)°; 4d : space group P2₁/c, Z = 4, a = 955,2(2) pm, b = 3190,9(4) pm, c = 930,7(2) pm, β = 99,64(1)°).     

Synthese einiger 1,2-Dihalogen-norbornane

Synthesis of some 1,2-Dihalogenonorbornanes The synthesis of 1,2exo-Dibromo-norbornane as well as the preparation of the configurational isomers of 2-bromo-1-iodo- and 2-chloro-1-iodo-norbornane are described.