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Contribution to the Chemistry of Trifluoromethylmercury (II) Compounds CF3HgI (I) has been obtained in appreciable amount by a newly modified method, The reaction of I with silver salts AgX or AgY2 (X = CN, NCO, SCN, SeCN, N3, SCF3, IO3; Y = O, C2O4, NCN) gives corresponding CF3HgX derivatives (II–VIII, XI, XII, XVII) mostly in good yield. The synthesis of (CF3Hg)2S (IX) has been attained by the reaction of I with Tl2CS3, while it gives with Ag2O (CF3Hg)2O (VIII) instead of the hydroxide. VIII reacts in ethereal solution with H2Se giving (CF3Hg)2Se (X). Stable CF3HgN and (CF3Hg)2N derivatives (XIII–XVII) could only be obtained when at least one more substituent on N atom, which reduces its basicity, is present. I.r., 19F-n.m.r. and mass spectroscopic data for the prepared compounds have been reported. 相似文献
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Contributions to the Chemistry of Transition Metal Diolefin Complexes. II. Characterization of Phosphine-stabilized Iron Diolefin Complexes Bis(butadiene)triphenylphosphine iron and Bis(isoprene)triphenylphosphine iron are characterized by protolytic reactions, mass spectrometrical fragmentations and NMR-spectra. A structure for this compounds is proposed on the basis of the NMR spectra. 相似文献
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Contributions to the Chemistry of Transition Metal Alkyl Compounds. XXXII. On Benzyl Copper Compounds Benzyl copper is formed reacting copper dichloride or acetylacetonate with dibenzyl zinc complexed by chlorides or acetylacetonates of copper and zinc. The complexes decompose between ?15 and +25°C with separation of copper and benzyl radicals proved by spin trap experiments. The stability of the compound is not influenced remarkably by substituents in o-position but is caused by complex formation with triphenyl phosphine. Pure benzyl copper, obtained by decomposition of BzCu · 0.25 BzZn(acac) · 0.75 Zn(acac)2 by means of diethyl ether, decomposes spontaneously even at a temperature of ?50°C. 相似文献
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Chemistry of Silicon-Nitrogen Compounds. 163. Investigation of Some Compounds with BNSi Structure Fragments Some formerly unknown compounds with BNSi structure fragments were prepared (or obtained on a not expected way), confirmed in their structure and described in their properties: (EtO)2BN(SiMe3)2 ( V ), FB[N(SiCl3)2]2 ( XIII ), the derivatives IV, XVI – XIX of the six-, five- and four-membered ring systems cyclotriazatriborane, cyclodisilaboradiazane, and cyclosilaboradiazane and XXIII of a [3, 4]-spiro system. Br2BN(SiMe3)2 ( III ), already known, was prepared by a different method. 相似文献
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Contributions to the Chemistry of Transition Metal Alkyl Compounds. XL. About Lithium Alkenylmanganates(II) MnCl2 reacts with vinyl, 2,2-dimethylvinyl, allyl, and methallyl lithium giving rise to alkenyl manganates(II). In a pure state the compounds Li2[Mn(CH?CH2)4] · 1.5 diox, Li2[Mn(CH?C(CH3)2)4] · 1.5 diox, Li2[Mn(CH2? CH?CH2)4] · 2.5 diox and Li3[Mn(CH2? C(CH3)?CH2)5] · 2 diox were isolated. The compounds were characterized by elementary analysis, EPR and IR spectra, magnetic moments, and reactions with iodine. 相似文献
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Contributions to the Chemistry of Sulfur Halides. 7. Trifluoromethyliodosulfane The preparation of CF3SI is reported. The molecule is characterized by vibrational, nuclear magnetic resonance, UV/VIS, and mass spectra. CF3SI chemically behaves like the interhalogen compound ICl. At higher temperatures the compound completely decomposes in CF3SSCF3 and I2. 相似文献
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Decamethylcyclotetrasilazane (I) was prepared starting with 1,3-dichloropentamethyldisilazane (II), 1.3-dichlorotetramethyldisilazane (III) and 1,3-bis-(methylamino)tetramethyldisilazane (IV). respectively, according to scheme 1, equ. (1), (2) and (3) in the text. (I) does not form, as given in the literature (equ. 4)5, by thermal transformation of bis(methylaminodimethylsilyl)-tetramethylcyclodisilazane (V); in this case exclusively – in equ. (2) and (3) only in side steps – the reaction products are a mixture of N-methylcyclotrisilazanes (scheme 2, VI–IX). 相似文献
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Contributions to the Chemistry of Silicon-Sulphur Compounds. 44. Trialkoxysilylthio Derivatives of Permethylpolysilanes By reaction of (RO)3SiSH · NEt3 (R = i-Pr, t-Bu) with α,ω-Cl2(SiMe2)n (n = 1, 2, 3, 4, 6) or with 1-Cl(SiMe2)nMe (n = 2, 4) trialkoxysilylthio derivatives of polysilanes of the two series α,ω-(RO)3SiS(SiMe2)nSSi(OR)3 and 1-(RO)3SiS(SiMe2)nMe have been prepared. Some properties of obtained new compounds were given. The resistance of the Si? S bond on protolytic splitting has been characterized by half-life times of the alcoholysis reaction. 相似文献
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Contributions to the Chemistry of Silicon-Sulphur Compounds. XXVIII. Trimethylsilylderivatives of Trialkoxysilanethiols The reactions of trialkoxysilanethiols and their salts with trimethylchlorosilane and hexamethyldisilazane were investigated. The preparation of trimethyltrialkoxydisilthianes has been described. Some properties of the obtained compounds were given and about their silylation ability has been considered. 相似文献
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Contributions to the Chemistry of Transition Metal Alkyl Compounds. 63. Preparation and Crystal Structure of Tetramethyltitanium Tetrahydrofuran Me4Ti · 2THF 1 dissoziates partially in n-pentane. The formed Me4Ti · THF 2 could be isolated. According to X-ray structure determination the molecules of 2 have a trigonalbipyramidal shape with the THF molecule in axial position. 相似文献
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Contributions to the Chemistry of Transition Metal Alkyl Compounds. XLIII. Tetrakis(alkoxycarbonylmethyl)titanium Compounds Organotitanium(IV) compounds of the type (ROCOCH2)4Ti (R ? C2H5, i-C3H7, t-C4H9, C6H5, C6H5CH2) were obtained by reactions of ROCOCH2Li derivatives with TiCl4 at low temperature. The compounds which decompose only above 90°C were characterized by the hydrolysis products, anaerobic reactions with iodine, and the i.r. spectra. The bond conditions are discussed. 相似文献
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Contributions to the Chemistry of Silicon-Sulphur Compounds. XXIX. 29Si-N.M.R. Investigations Three series of silicon-sulphur compounds (RO)3SiSR′ (I), (i-PrO)4?nSi(SEt)n (II) and cyclic Si? S compounds (III) were prepared, some of them at the first time and their 29Si-N.M.R. spectra were measured. In the series of trialkoxysilylthio derivatives (I) were the steric and inductive effects of the RO and R'S groups evaluated. In the series II were the 29Si-N.M.R. chemical shifts related to the relative paramagnetic screening constants σ* and netto charge at the silicon atom q(Si) using the EN-quantum-chemical model discussed. In the series III were the shift contribution of the (SiS)2 and 1-sila-2,5-dithiacyclopentan rings determined. 相似文献
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Contributions to the Chemistry of Transition Metal Alkyl Compounds. XXXVIII. Reactions of Dibenzyl Manganese with Oxygene (C6H5CH2)2Mn · C4H8O2 reacts with oxygen forming an unstable deep violet compound which changes in a stable unsoluble yellow peroxide of the formula C6H5CH2MnO? OMnCH2C6 H5. With excess oxygen a polynuclear complex of 3 valent manganese is formed with the composition Mn4O4(OH)4(OCHC6H5)2. The compounds isolated were characterized by the products of hydrolyses and thermolyses, anaerobic reaction with iodine, magnetic moments, i.r. and e.s.r. spectra. 相似文献
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Contributions to the Chemistry of Transition Metal Alkyl Compounds. XV Preparation and Properties of Phenyl Vanadium Dichloride Vanadium(IV) chloride reacts with diphenyl zinc forming extremely air sensitive, at room temperature stable phenyl vanadium dichloride. The diffuse reflectance spectrum indicates an octahedral structure of the vanadium compound which is to regard as a coordination polymer. – Diethyl ether causes a cleavage of the V – C bond with formation of a vanadium dichloride etherate. 相似文献
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Walter Fink 《Helvetica chimica acta》1969,52(7):1833-1841
Linear oligosiloxanes with cyclodisilazane rings built into the siloxane chain were prepared by the reaction of hydroxysilyl substituted cyclodisilazanes in the form of their lithiumsilanolates with dimethyldichlorosilane, α,ω-chlorosiloxanes or dimethylchlorosilyl substituted cyclodisilazanes. 相似文献
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Contributions to the Chemistry of Transition Metal Alkyl Compounds. XLI. Preparation and Thermolysis Products of Methyl Titanium Halides (CH3)nTiX4 ? n derivatives (X = Cl, Br, I) can be prepared by comproportionation reactions of tetramethyl titanium with titanium tetrahalides at deep temperature. Furthermore, the methyl titanium iodides are formed from tetramethyl titanium and iodine. Thermolysis of CH3TiX3 derivatives yields titanium(III) halides. At decomposition of the (CH3)2TiX2 compounds in ether solution titanium(II) halides are obtained in a fine-distributed, very reactive form. 相似文献
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Contributions to the Chemistry of Transition Metal Diolefin Complexes. III. Electro-chemical Preparation of Cobalt Complex Compounds of Noncyclic 1,3-Diolefins The synthesis is described of butadiene coordination compounds of the type (π-C4H6)Co(π-C4H6R) · L by electrolytic reduction of cobalt salts in presence of butadiene, where R represents an H or C4H7 radical and L P(n-C4H9)3 or P(C6H5)3. 相似文献