- Molecular and crystal structures of Cp*M(S2N2) (M = Co, Rh, Ir) and related compounds
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Cp*Rh(S2N2) was prepared as a microcrystalline solid by using [S4N3]Cl in liquid ammonia or [nBu 2Sn(S2N2)]2. It was characterised by NMR, IR and Raman spectroscopy an
- Matuska, Vit,Tersago, Karla,Kilian, Petr,Van Alsenoy, Christian,Blockhuys, Frank,Slawin, Alexandra M. Z.,Derek Woollins
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Read Online
- Preparation method of monobutyltin oxide
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The invention provides a preparation method of monobutyltin oxide. The method includes the steps of firstly, adding tetrabutyl tin into a reactor, evenly stirring, slowly dropwise adding tin tetrachloride, then stirring for 30 minutes, heating to 140 DEG C, and performing heat-preservation reaction for 4-8 hours to obtain the mixed solution of monobutyltin trichloride and dibutyltin dichloride; secondly, heating the mixed solution of the monobutyltin trichloride and the dibutyltin dichloride to 95-100 DEG C, and collecting the monobutyltin trichloride; thirdly, adding the monobutyltin trichloride collected in the second step, surfactant and an organic solvent into a reactor, evenly stirring, slowly dropwise adding a sodium hydroxide solution, then heating to 90 DEG C, performing heat-preservation reaction for 3.5-4 hours, cooling to room temperature, filtering to obtain crude monobutyltin oxide, washing the crude monobutyltin oxide until the crude monobutyltin oxide is neutral, and performing reduced-pressure drying at 80 DEG C for 12 hours to obtain the monobutyltin oxide, wherein the surfactant is chitosan modified imidazoline ampholytic surfactant and quaternized polyvinyl alcohol.
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Paragraph 0068; 0070; 0071; 0085-0155
(2017/08/29)
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- Preparation method of dibutyltin oxide
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The invention provides a preparation method of dibutyltin oxide. The dibutyltin oxide is at least prepared by (1), synthesis of tetrabutyl tin; (2), synthesis of dibutyl stannous chloride; (3), synthesis of dibutyltin oxide, wherein catalyst used in step (2) is composite of modified nano-crystalline cellulose and aluminium chloride. The dibutyltin oxide is applied to electric paint and electrophoretic paint fields.
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Paragraph 0069; 0072; 0083-0104; 0110-0131; 0137-0149
(2017/09/05)
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- PREPARATIONS OF META-IODOBENZYLGUANIDINE AND PRECURSORS THEREOF
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The present disclosure provides purified forms of iobenguane and preparations of a precursor to iobenguane, such as a polymer, the polymer comprising a monomer of formula (I) or a pharmaceutically acceptable salt thereof, the preparation comprising leachable tin at a level of 0 ppm to 850 ppm.
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- Indium-mediated regioselective synthesis of ketones from arylstannanes under solvent-free ultrasound irradiation
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The solvent-free indium-promoted reaction of alkanoyl chlorides with sterically and electronically diverse arylstannanes is a simple and direct method for the regioselective synthesis of primary, secondary and tertiary alkyl aryl ketones in good to excellent isolated yields (42-84%) under mild and neutral conditions. The protocol is also adequate for the synthesis of aryl vinyl ketones. Reaction times are drastically reduced (from 3-32 h to 10-70 min) under ultrasonic irradiation. Evidences for the involvement of a homolytic aromatic ipso-substitution mechanism, in which indium metal acts as radical initiator, are presented. It is possible the transference of two aryl groups from tin, thus improving effective mass yield, working with diarylstannanes as starting substrates.
- Lo Fiego, Marcos J.,Badajoz, Mercedes A.,Domini, Claudia,Chopa, Alicia B.,Lockhart, María T.
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p. 826 - 832
(2013/03/14)
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- Tri- and diorganostannates containing 2-(N,N-dimethylaminomethyl)phenyl ligand
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The C,N-chelated tri and diorganotin(IV) chlorides react with both protic mineral acids and carboxylic acids. The nitrogen atom of the LCN ligand (where LCN is 2-(dimethylaminomethyl)phenyl) is thus quarternized - protonated and new Sn-X bond (X = Cl, Br, I or the remainder of the starting acid used) is simultaneously formed. The set of zwitterionic tri and diorganostannates containing protonated 2-(dimethylaminomethyl)phenyl-moiety was prepared and structurally characterized by multinuclear NMR spectroscopy and XRD techniques. In all these cases, the intramolecular N-H?X bond is present in the molecule. Despite the central tin atom remains five-coordinated (except for the [HLCNH]+[(n-Bu)2SnCl(NO 3)2]-) and reveals a distorted trigonal bipyramidal geometry, the 119Sn NMR chemical shift values of these zwitterionic stannates are somewhat shifted to the higher field than corresponding starting C,N-chelated tri and diorganotin(IV) halides. Reactions of C,N-chelated organotin(IV) halides with various Lewis acids are also discussed.
- ?vec, Petr,?erno?ková, Eva,Padělková, Zdeňka,R??i?ka, Ale,Hole?ek, Jaroslav
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p. 2475 - 2485
(2010/11/16)
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- Five-membered arsenic-sulfur-nitrogen heterocycles, RAs(S2N 2) (R = Me, Et, iPr, tBu, Ph, Mes)
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A series of 5-alkyl/aryl-1,3λ4δ2,2,4,5- dithiadiazarsoles RAs(S2N2) (R = Me, Et, iPr, tBu, Ph, Mes) were prepared by a ligand exchange between [ nBu2Sn(S2N2)]2 and the corresponding organodihalogenoarsines RAsX2 (X = Cl, I). All products were characterized by NMR, IR, and Raman spectroscopies and mass spectrometry. The crystal structures of the aryldithiadiazarsoles (R = Ph, Mes) were determined.
- Matuska, Vit,Slawin, Alexandra M. Z.,Derek Woollins
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p. 3064 - 3069
(2010/06/14)
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- PROCESS FOR PRODUCTION OF DIALKYLTIN DIALKOXIDES
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An object of the present invention is to provide a process for producing a dialkyl tin compound from a composition of deactivated forms of a dialkyl tin catalyst, and to provide a process for producing the dialkyl tin catalyst from the dialkyl tin compound and using the dialkyl tin catalyst to produce a carbonic acid ester. According to the present invention, a process for producing a dialkyl tin compound is provided that subjects a composition of the deactivated forms of the dialkyl tin catalyst, formed when producing an ester compound, to an alkyl group redistribution reaction and/or dealkylation reaction.
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Page/Page column 36
(2009/07/25)
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- Synthesis, structures, and properties of mixed dithiolene-carbonyl and dithiolene-phosphine complexes of tungsten
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A new, high yield synthesis of [Ni(S2C2Me 2)2] (3) is described using 4,5-dimethyl-1,3-dithiol-2-one, Me 2C2S2C=O (1), as dithiolene ligand precursor. Reaction of (Me2C2/su
- Chandrasekaran,Arumugam, Kuppuswamy,Jayarathne, Upul,Perez, Lisa M.,Mague, Joel T.,Donahue, James P.
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p. 2103 - 2113
(2009/07/18)
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- Process for the preparation of monoalkyl tin trihalides and dialkyl tin dihalides
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The present invention comprises a process for the production of monoalkyltin trihalides of the formula RSnHal 3 , in which R = alkyl or cycloalkyl and Hal = Cl, Br or I, said process comprising contacting alkene, stannous halide and hydrogen halide in the presence of at least one transition metal complex as a catalyst or catalyst precursor; optionally thereafter isolating the monoalkyltin trihalides from the medium. Advantageously M is selected from Group VIII of the periodic Table of elements. The reaction can be carried out with or without a solvent. The reaction proceeds selectively, the only significant side product being alkene isomers resulting from isomerisation of the starting alkene. The alkene is currently applied in excess to the other reactants. The hydrogen halide acid may be employed as gas or in solution. The reaction proceeds smoothly at room temperature or above. A multitude of organic solvents can be used, in particular, solvents like alcohols, ethers and apolar aromatic and aliphatic solvents and mixtures thereof. Small amounts of water do not disturb the reaction. The invention also comprises a process to make dialkyltin dihalides. The monoalkyltin trihalides (i) either isolated from the above reaction medium (ii) either coming from another source are reacted with tin metal to get a mixture of tin dihalide and dialkyltin dihalides. Optionally in option (i) the tin metal can be added during the reaction to monoalkyltin trihalide. In that way the tin dihalide formed can be consumed to produce monoalkyltin trihalide. The invention also relates to the use of these monoalkyltin trihalides, dialkyltin dihalides and mixtures thereof made according to the process hereabove as intermediates for PVC stabilisers, glass coating Chemicals and catalysts.
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Page/Page column 6
(2008/06/13)
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- Can mono- or di-butyltin chlorides produce tributyltin chloride at elevated temperatures? Implications for applications in chemical vapour deposition
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The thermolysis of the butyltin chlorides at 200-300 °C in the liquid phase has been investigated by 1H, 13C, and 119Sn NMR spectroscopy. The stabilities follow the order: Bu2SnCl2 > Bu3SnC
- Davies, Alwyn G.,Sella, Andrea,Sivasubramaniam, Rajaveen
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p. 3556 - 3561
(2007/10/03)
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- Synthesis of novel terdentate N,C,N′-coordinated butyltin(IV) complexes and their redistribution reactions with SnCl4
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The Sn(IV) butyl complexes [BunSnCl3 - n(NCN)] (NCN = [C6H3(CH2NMe2)2-2,6] -, n = 1 (1), 2 (2), 3 (3)) were prepared. Spectroscopic analysis of 1-3 by 1H and 119Sn NMR gave evidence for the presence of intramolecular N → Sn interactions in solution. The molecular structure of 1, as determined by a single-crystal X-ray diffraction study, revealed that it contained a six-coordinate Sn(IV) center with intramolecular N → Sn coordination of both ortho-amine substituents. Addition of SnCl4 to 1 resulted in the isolation of the HCl adduct [BuSnCl3(NCN +H)] (6). Reactions of 2 and 3 with SnCl4 each resulted in the HCl salt [SnCl4(NCN+H)] (8) and the corresponding butyltin chloride, Bu2SnCl2 and Bu3SnCl, respectively. The formation of HCl adducts 6 and 8 was ascribed to transfer of the NCN ligand to SnCl4 and the presence of HCl (from partial hydrolysis of the product or SnCl4 during the work up procedure). The molecular structures of 6 and 8 have been determined through single-crystal X-ray diffraction and revealed the presence of a [BuSnCl3(aryl)] - or [SnCl4(aryl)]- stannate anion, respectively, with in each case one coordinated ortho-amine function and one protonated amine moiety involved in N-H?Cl-Sn hydrogen bonding in both compounds (2.14 ? for 6 and 2.18 ? for 8).
- Thoonen, Sander H.L.,Van Hoek, Hein,De Wolf, Elwin,Lutz, Martin,Spek, Anthony L.,Deelman, Berth-Jan,Van Koten, Gerard
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p. 1544 - 1553
(2007/10/03)
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- A new way to scorpionate niobium complexes: Terminal alkyne, imido, and oxo complexes and the rearrangement of α-agostic ethyl complexes
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Synthesis of new hydrotris(pyrazolyl)-borate(Tp′) niobium terminal alkyne complexes and some reactions of these complexes was investigated. THF and diethyl ether were obtained after refluxing purple solutions of Na/benzophenone under dinitrogen. Deuterated nuclear magnetic resonance (NMR) solvents were dried over molecular sieves, degassed by freeze-pump-thaw cycles, and stored under dinitrogen. The thermoanalysis suggested that reversible migratory insertion yield hydride complexes, although the stability of these complexes has precluded a detailed investigation of the reaction course.
- Oulie, Pascal,Brefuel, Nicolas,Vendiez, Laure,Duhayon, Carine,Etienne, Michel
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p. 4306 - 4314
(2008/10/09)
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- Efficient Synthesis of Salts of the Tetrakis(perfluoroorgano)borate anion, [B(CF=CF2)4]-
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The synthesis and the NMR spectra of the tetrakis(trifluorovinyl)borate salts M[B(CF=CF2)4] (M = Li, K, Cs, [NR1R 32) as well as the X-ray crystal structure of the tetramethylammonium salt are reporte
- Adonin, Nicolay Yu.,Bardin, Vadim V.,Floerke, Ulrich,Frohn, Hermann-Josef
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p. 172 - 174
(2008/10/09)
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- Synthesis of Aromatic and Olefinic Sodium Sulfonates by Electrophilic Destannylation with Trimethylsilyl Chlorosulfonate
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A mild and effective method for the preparation of a variety of aromatic, olefinic, and acetylenic sodium sulfonates is described.The reaction of trialkylaryl- (2a-k) and -heteroarylstannanes (4a-d), bis-(1-alkenyl)dibutylstannanes (6a-f), or trialkylakynylstannanes with trimethylsilyl chlorosulfonate (1) followed by hydrolysis with aqueous NaHCO3 provides the sodium sulfonates in an ipso-specific and in the case of vinylic stannanes stereospecific manner.A comparision of the reactivity of stannylated and silylated olefinic compounds 13 and 14 underlines the greater leaving ability of the stannyl moiety.The in situ preparation of the stannanes makes it possible to apply the synthetic method to natural products such as N-substituted apocodeine (17). - Key Words: Electrophilic aromatic substitution/ Electrophilic vinylic substitution/ Trialkylstannanes, application of/ Arylsulfonates, sodium salts of/ Vinylsulfonates, sodium salts of
- Niestroj, Michael,Lube, Andreas,Neumann, Wilhelm P.
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p. 575 - 580
(2007/10/02)
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- Refining process of organic tin (IV) polyhalides
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It is possible to eliminate organic tin(IV) monohalide from organic tin(IV) polyhalide containing the monohalide so that it can not be detected in sensitivity of ordinary gas chromatography by treating with hydrochloric acid, hydrogen chloride or chlorine.
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- Synthesis and properties of isocyanate and isothiocyanate d1- and d2-complexes of vanadocene
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The reactions of vanadocene and its halides Cp2VCl and Cp2VCl2 with R3MNCX (M = Sn, Si, X = O, S) and R2M(NCX)2 in various molar ratios have been studied.The reactions proceed either by an exchange of groups, with no change in the oxidation state of vanadium, or by an oxidative addition of pseudohalide ligand: VII -> VIII; VIII -> VIV.Oxidative addition results in the formation of (R3M)2 or gaseous hydrogen (in the reaction with HCl) in the reaction products.We have prepared the first ever monomeric and readily oxidisable d2-complexes of VIII of Cp2VNCX-type and asymmetric d1-complexes of Cp2V(Cl)NCX type, which, although rather stable in air, undergo disproportionation into symmetric d1-complexes on heating.In transmetallation reactions the ligand activity is found to increase in the order Cl A general scheme for the disproportionation reaction of asymmetric complexes of vanadocene is supported by differential thermal analysis data.
- Razuvaev, G. A.,Gordetsov, A. S.,Latyaeva, V. N.,Zimina, S. V.,Skobeleva, S. E.,et al.
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p. 327 - 336
(2007/10/02)
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- A highly selective synthesis of R2SnX2 (R = alkyl, X = Br, Cl) species directly from tin and alkyl halides
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The reaction : Sn + 2RX -> SnR2X2 (X = Cl, Br) occurs at relatively low temperature (80 - 120 degC) and with selectives as high as 95 - 99percent in the presence of catalytic system fored by a crown ether and potassium iodide.The reaction is favoured by aprotic dipolar solvents such as dimethylformamide; the presence of an alkyl iodide as cocatalyst has a positive effect, the selectivity remaining unchanged.
- Ugo, R.,Chiesa, A.,Fusi, A.
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- β-SUBSTITUTED ALKYLTIN HALIDES. III. SYNTHESIS OF TRIALKYLTIN HALIDES AND TETRAALKYLTINS
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(β-Carboalkoxyethyl)tin trihalides and bis(β-carboalkoxyethyl)tin dihalides react with metallic zinc to give mixtures of the corresponding tris(β-carboalkoxyethyl)tin halides and the tetra(β-carboalkoxyethyl)tins.Bis(β-carboalkoxyethyl)tin diacetates react with metallic zinc to give only the corresponding tetra(β-carboalkoxyethyl)tin compounds.The mechanisms of these reactions are discussed.Conversion of the bis(β-carboalkoxyethyl)tin dihalides into the tris(β-carboalkoxyethyl)tin halides is believed to occur by a two-step process, with the tetra(β-carboalkoxyethyl)tin compounds as intermediate products.The 270 MHz NMR spectra of the (β-carbobutoxyethyl)tin compounds are presented.
- Burley, Joseph W.,Hutton, Ronald E.,Jolley, Michael R.J.,Groenenboom, Cornelis J.
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p. 189 - 202
(2007/10/02)
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- Reactions of Thionyl Chloride with Tetraorganotin(IV) Compounds
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The reactions of thionyl chloride with tetraorganotin(IV) derivatives (R4Sn where R = CH3, C2H5, n-C3H7, n-C4H9, C6H5CH2, C6H4CH3) bring about cleavage of tin-carbon bonds to give dialkyl/aryltin(IV) and alkyl/aryl sulphinyl chlorides.The ease of cleavage observed on the basis of the reactivities of R4Sn follows the order: n-C4H9 > n-C3H7 > C2H5 > CH3 > C6H5CH2 >> C6H4CH3.This order is not the same as commonly known in literature.
- Narula, Suraj P.,Sharma, R. K.,Lata, Sneh,Walia, Rita
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p. 246 - 247
(2007/10/02)
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- INVESTIGATION OF THE DIRECT SYNTHESIS OF TETRABUTYLTIN FROM BUTYL CHLORIDE
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The direct synthesis of tetrabutyltin from butyl chloride, has been investigated, and the various contributing reactions have been identified.A mechanism is proposed for the overall synthesis, which comprises radical-ionic processes for the liberation of metal atoms from the surfaces of the metal powders, followed by formation of bridging intermediates leading to the transfer of butyl groups from zinc to tin, until the synthesis of tetrabutyltin is complete.Although dibutyltin dihalides were shown to be probable intermediates in the process, the known organohalostannate complex Bu4N+ - was not found to be formed under the conditions used.
- Nicholson, John W.,Douek, Josephine A.,Collins, John D.
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p. 173 - 183
(2007/10/02)
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- REDISTRIBUTION REACTIONS OF β-CARBOALKOXYETHYLTIN COMPOUNDS
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Carboalkoxyethyltin compounds undergo redistribution reactions at faster rates than similar unsubstituted alkyltin compounds.In redistribution reactions between SnCl4 and carboalkoxyethyltin compounds stable intermolecular complexes are formed.Rate enhancement is explained in terms of intra- and intermolecular coordination effects.Where strong intermolecular coordination effects are observed, specific electrophilic cleavage of the carboalkoxyethyl group can occur in preference to alkyl cleavage in mixed carboalkoxyethylalkyltin compounds.The presence of a β-ester function can catalyse both alkyl/chlorine and alkyl/alkyl' exchange reactions.
- Burley, Joseph W.,Hutton, Ronald E.
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p. 165 - 176
(2007/10/02)
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- A NOVEL SYNTHETIC ROUTE TO DIORGANOTIN DICHLORIDES AND DIBROMIDES
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Diorganotin dichlorides and dibromides can be prepared by a simple and convenient one-step process involving the reaction of Grignard reagent with (Acac)2SnX2 (Acac H = pentane-2,4-dione; X = Cl or Br).The yields of lower diorganotin dihalides are excellent while those of higher diorganotin dihalides are moderate.
- Chandrasekaran, R. K.,Venkataraman, S.,Koola, Johnson D.
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p. C43 - C44
(2007/10/02)
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- DERIVATIVE DES BOROLS II. PENTAPHENYLBOROL: SYNTHESE, REDUKTION ZUM DIANION UND KOMPLEXE VON KOBALT UND PLATIN
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Analytically pure, dark blue pentaphenylborole (PPB) can be synthesized from 1,1-dibutyl-2,3,4,5-tetraphenylstannole and C6H5BCl2 in toluene in 95percent yield.Reduction of PPB with elemental potassium in THF produces brownish red K2 which is derived from the new 6?-electron anion 2-.The new complexes (C5H5)Co(PPB) and (COD)Pt(PPB) (COD=1,5-cyclooctadiene) are obtained by irradiation of a toluene solution of (C5H5)Co(CO)2 and PPB and by ligand substitution reaction from Pt(COD)2 and PPB respectively.
- Herberich, G. E.,Buller, B.,Hessner, B.,Oschmann, W.
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p. 253 - 260
(2007/10/02)
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- Process for preparing organotin compounds
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Tricycloalkyltin chlorides e.g. tricyclohexyltin chlorides, which may be converted to the fungicide tricyclohexyl hydroxide, are made by reacting an organic tricycloalkyltin, in which the organic is not cycloalkyl and cycloalkyl is optionally substituted cyclohexyl, with organic tin trihalide.
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