Synthese und Eigenschaften einigerp-tolyl-phenylsubstituierter Di- und Trisilane und von 1,1,1,3,3,3-Hexaphenyltrisilan

The synthesis and properties of [Ph ₂ p-TolSi]₂, [Ph ₂ p-TolSi]₂SiPh ₂, [Ph ₃ Si]₂Si(p-Tol)₂, [Ph ₂ p-TolSi]₂Si(p-Tol)₂ and (SiPh ₃)₂SiH₂ are described. The silanes are identified using IR,Ra- and²⁹Si-NMR-spectroscopy.

     

Intra- und intermolekulare elektronische und Schwingungsrelaxation

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Nachweis und Bestimmung von Hydrastin und Berberin in Drogen und Extrakten

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Physikalische und physikochemische Mikromethoden und -apparate

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Acyclische und cyclische Silylhydrazone und Hydrazonylsilane

Acyclic and Cyclic Silylhydrazones and Hydrazonylsilanes Dimethylketone-di-tert-butylmethylsilylhydrazone ( 1 ) is obtained in the reaction of the silylhydrazine and dimethylketone by condensation. Di-tert-butyldifluorosilane reacts with lithiated hydrazones to give fluorosilylhydrazones 2–4 , (CMe₃)₂SiF? NH? N = CRR′, ( 2 : R=Me, R′=CMe₃; 3 : R,R′=CHMe₂; 4 : R,R′=Ph). The bis(hydrazonyl)silane 5 , (CMe₃)₂Si(NH? N=CPh₂)₂, is formed in a molar ratio 1:2. Tris( 6 )- and tetrakis(hydrazonyl)silanes ( 7 ) are obtained from CMe₃SiF₃ ( 6 ), SiF₄ ( 7 ), and lithiated tert-butylmethylketon-hydrazone. The lithium derivatives 8–11 are formed in the reaction of 1–4 with butyllithium. Bis(silyl)hydrazones ( 12–15 ) are the result of the reaction of halogensilanes and the lithium derivatives of 1(8), 2(9) and 3(10); 12 : (CMe₃)₂SiMe(CMe₃SiF₂)-N? N=CMe₂, 13 : (CMe₃)₂MeSi(PhSiF₂)N? N=CMe₂, 14 : (CMe₃)₂SiF(Me₃Si)N? N=C(Me)(CMe₃), 15 : (CMe₃)₂SiF (SiMe₃)N? N=C(CHMe₂)₂. Saltelimination out of 10 und 11 leads to the formation of the first bis(imino)-2,2,4,4-cyclodisilazanes, 16 :[(CMe₃)₂ SiN? N=C(CHMe₂)₂]₂, 17 : [(CMe₃)₂SiN? N=CPh₂]₂. Cyclisation occurs in the reaction of 12 und 14 with tert-butyllithium, 2-silyl-1,2-diaza-3-sila-5-cyclopentenes ( 18 and 19 ) are formed. Dilithiated 1 reacts with SiF₄ to give the spirocyclic compound 20 . HF-elimination from 18 and dimerisation of the intermediate diazasilacyclopentadiens lead to the formation of the tricyclus 21 .     

Herstellung und Charakteristika von o-Acryloyloxy- und o-Methacryloyloxybenzoes?ure und ihren Polymeren

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Titan und Eisen in Titan-, Eisen- und Zirkoniumerzen und -konzentraten

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Darstellung und strukturuntersuchungen von dimethylmetallacet- und acetimidohydrazinderivaten des galliums und indiums

Trimethylgallium and trimethylindium react with N′,N$\text{-}\text{?}$ dimethylacethydrazine and N′,N″,N′″-trimethylacetimidohydrazine, respectively, to form as a first step, monomeric dimethylmetal derivatives with five-membered ring skeletons. These heterocyclic compounds immediately add a further alkylmetal molecule. The ¹H NMR, IR and Raman spectra of these compounds are discussed and the results of X-ray structure determinations of two of the adducts are given.     

Synthese und Charakterisierung von Fluorenylgallaten und Fluorenylindaten

Synthesis and Characterization of Fluorenyl Gallates and Fluorenyl Indates GaCl₃ reacts with Fluorenyllithium (LiFl) in the ratio 1:4 in Et₂O to [Li(THF)₄][GaFl₄] ( 1 ). The addition of DME (1,2-dimethoxyethane) to solutions of 1 in THF leads to [Li(DME)₃][GaFl₄] ( 2 ) under replacement of THF molecules by DME molecules in the coordination sphere of the Li⁺ ions. Treatment of InCl with LiFl in Et₂O and recrystallization from THF gives [Li(THF)₄][ClInFl₃] ( 3 ), which is formed by an disproportionation reaction. 3 can also be obtained by the reaction of InCl with FlZnCl/LiCl in Et₂O and recrystallization from THF. 1 and 2 crystallize from THF and THF/DME as [Li(THF)₄][GaFl₄] · THF ( 1 · THF) and [Li(DME)₃][GaFl₄] · THF ( 2 · THF), respectively. Crystalline 3 is isolated from the reaction of InCl and FlZnCl/LiCl, while the reaction mixture of InCl and LiFl gives after recrystallization in THF 3 · 1,5 THF. The gallate ions in 1 and 2 differ mainly in the position of the fluorenyl ligands. The unit cells of 3 and 3 · 1,5 THF contain two crystallographic unique ion pairs of [Li(THF)₄][ClInFl₃].     

Komplexe von Acetylaceton und Acetonylaceton mit Alkali- und Erdalkaliionen. MO-SCF-Berechnungen und UV-Spektroskopie

In analogy to previous investigations on main group metal ion complexes with diacetyl², model calculations within the LCGO MO SCF framework using minimal basis sets are used in combination with UV spectrocopy in order to investigate complex formation tendencies, eventual ion specifities and ion binding energies of Li, Na, K, Mg and Ca ions with dicarbonyl ligands. The influence of the separation of the coordinative centers by methylene groups on the interaction with these metal ions is discussed. The simple quantum chemical models seem to work in the case of diacetyl and acetylacetone, whereas they fail in the prediction of the experimentally observed interaction of acetonylacetone with the metal ions.

     

Trennung und Bestimmung von Antimon und Zinn

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