Antimony Pentachloride Complex Research Articles

ChemInform Abstract: Reactions of Tetrasulfur Tetranitride Antimony Pentachloride Complex (S4N4SbCl5) with Primary β-Enaminones and β-Enamino Esters: Synthesis of 4-Substituted 3-Aroyl- and 3-Ethoxycarbonyl-1,2,5-thiadiazoles.

ChemInform Abstract: Reactions of Tetrasulfur Tetranitride Antimony Pentachloride Complex (S4N4SbCl5) with Primary β-Enaminones and β-Enamino Esters: Synthesis of 4-Substituted 3-Aroyl- and 3-Ethoxycarbonyl-1,2,5-thiadiazoles.

A Stepwise Synthesis of Bi-1,2,5-thiadiazole Compounds Using S4N4·SbCl5 Complex

Bi-1,2,5-thiadiazole compounds (7) were synthesized step by step by reaction of 1-(4-substituted-3-1,2,5-thiadiazolyl)alkanone oximes (6) with tetrasulfur tetranitride antimony pentachloride complex (S 4 N 4 SbCl 5 , 1) in toluene at 100 °C for 0.5 h in 28 - 80% yields.

Reactions of Tetrasulfur Tetranitride Antimony Pentachloride Complex (S4N4·SbCl5) with Primary b-Enaminones and b-Enamino Esters: Synthesis of 4-Substituted 3-Aroyl- and 3-Ethoxycarbonyl-1,2,5-thiadiazoles

Reactions of Tetrasulfur Tetranitride Antimony Pentachloride Complex (S4N4·SbCl5) with Primary b-Enaminones and b-Enamino Esters: Synthesis of 4-Substituted 3-Aroyl- and 3-Ethoxycarbonyl-1,2,5-thiadiazoles

ChemInform Abstract: Reactions of Alkyl Methyl Ketoximes with Tetrasulfur Tetranitride Antimony Pentachloride Complex (S4N4×SbCl5): A Regioselective Formation of 3‐Alkyl‐4‐methyl‐1,2,5‐thiadiazoles and Their Mechanism of Formation.

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Reactions of Alkyl Methyl Ketoximes with Tetrasulfur Tetranitride Antimony Pentachloride Complex (S4N4ÅESbCl5): A Regioselective Formation of 3-Alkyl-4-methyl-1,2,5-thiadiazoles and Their Mechanism of Formation

Reactions of Alkyl Methyl Ketoximes with Tetrasulfur Tetranitride Antimony Pentachloride Complex (S4N4ÅESbCl5): A Regioselective Formation of 3-Alkyl-4-methyl-1,2,5-thiadiazoles and Their Mechanism of Formation

Reactions of 5-substituted 3-alkyl- and 3-aryl-isoxazoles with tetrasulfur tetranitride antimony pentachloride complex (S4N4·SbCl5): complete regioselective formation of 4-substituted 3-acyl- and 3-aroyl-1,2,5-thiadiazoles and their mechanism of formation

The reactions of 3-alkyl- 5a–f, 3-aryl- 5g–m, 3-acylamido- 5n,p, 3-benzamido- 5o and 3-arylamino- 5q -5-alkyl- and -5-aryl-isoxazoles with tetrasulfur tetranitride antimony pentachloride complex (S4N4·SbCl5) in toluene at 90 °C to reflux temperature give 3-acyl- 6a–c, e, n–q and 3-aroyl-4-substituted-1,2,5-thiadiazoles 6d, f–m in 13 to 61% yields as single isomers. The same reactions of 3,4-dimethyl- 5s, 5v, 4-ethyl-3-methyl- 5t -5-alkyl- and/or 5-aryl-isoxazoles under the same conditions give 3-(1-acetyl-1-chloroethyl)- 8a, 3-(1-benzoyl-1-chloropropyl)- 8b, 3-(1-benzoyl-1-chloroethyl)- 8d, or 3-(1-benzoyl-1-chloroethyl)-4-methyl-1,2,5-thiadiazoles 8c, which are a new type of 1,2,5-thiadiazole derivatives. In addition the reactions with 5-aryl-4-bromoisoxazoles (5,w,y,z) having an electron-donating substituent such as methyl, 4-methylphenyl, and 4-methoxyphenyl groups at C3 under the same conditions afford 3-aroyl-4-substituted-1,2,5-thiadiazoles 6d, 6j and 6k, whereas the starting isoxazoles are recovered from the reactions with 5-aryl-4-bromoisoxazoles 5x,z′ having a phenyl or a 4-chlorophenyl group at C3. A plausible mechanism is proposed for the formation of the products.

Living polymers from cyclodimethylsiloxanes through non-protonic initiation

Complexes of antimony pentachloride with acyl chlorides such as acetyl chloride or 1-naphthoyl chloride polymerize various completely methylated cyclosiloxanes such as hexamethylcyclotrisiloxane (D3) or dodecamethylcyclohexasiloxane (D6) with high rates of initiation and propagation, their activity being unchanged in the presence of the proton-trap 2,6-di-tert-butyl-4-methylpyridine. For polymerization of D3 conducted at −10°C in methylene dichloride, there is a simultaneous and proportional formation of high-molecular-weight polymer (HP), of small cycles of the D3x type (concentrations [D6] > [D9] > [D12] > …) and of macrocycles. A linear increase of the molecular weight (M) of HP is observed up to at least 50% conversion, in agreement with the presence of a constant number of macromolecules of high molecular weight, mainly consisting of a living polymer population. For higher conversions, M may grow more rapidly which may be explained by an increasing copolymerization of D6 and D9 with D3. Homopolymerization of D6 occurs under similar conditions with a rate smaller than that for D3, but also with linearly increasing M of HP with conversion. The simultaneous formation of the various products is attributed to the presence of two populations of macromolecules. One of these would bear either two active centres or one active centre and one non-reacting end-group, and the other population would bear one active centre and one reacting end-group, giving by end-to-end ring closure, macrocycles and eventually smaller cycles.

Synthesis and spectroscopic study of complexes of antimony pentachloride with some benzonitrile derivatives

AbstractThe complexes SbCl5 · L (L = 2,3 and 4‐chlorobenzonitriles and 2,3 and 4‐aminobenzonitriles) have been isolated and investigated by conductivity and IR and Raman spectral measurement. From the IR spectra it is inferred that in all complexes, coordination of the ligands to the Sb takes place through the nitrogen atom of the nitrile group. In addition, the spectral data are in full accord with a molecular adduct of local C4v symmetry for the SbCl5N moiety.

Metal Complexes of Cyanamides and their Alkylation to Cyanamidium Salts. A General Synthesis of Highly Substituted Ureas, Isoureas, and Guanidines

AbstractThe complexes 3a – p were prepared from disubstituted cyanamides and Lewis acids. According to a X‐ray structural analysis, the antimony pentachloride complex 3a is neither a s̀ nor a π complex (∡ CN – Sb 133°). The complexes 3 with SbCl5 and FeCl3 can be alkylated with tertiary alkyl chlorides, affording crystalline cyanamidium salts (5a – m) which were characterized by reactions with water, primary or secondary alcohols to give ureas (11) and uronium salts (8a – z), respectively. The guanidinium salts 9a – s were obtained with ammonia, primary and secondary amines.

Vibrational spectroscopic study of some benzonitrile complexes of antimony pentachloride

Complexes of antimony pentachloride were prepared with benzonitrile, 2,3− and 4-methyl-benzonitriles, and 2,3−; 2,4−; 2,5− and 3,4-dimethylbenzonitriles of the type SbCl 5·L. All the isolated solids were non-electrolytes in nitromethane. The i.r. and Raman spectral data of the complexes are in good agreement with local C 4 v symmetry for the SbCl 5N moiety. A classification of the donor strength of benzonitriles is proposed.

ChemInform Abstract: NUCLEAR QUADRUPOLE RESONANCE AND STEREOCHEMISTRY. PART 7. THE AXIAL AND EQUATORIAL CHLORINE ATOMS IN OCTAHEDRAL COMPLEXES OF ANTIMONY PENTACHLORIDE, SBCL5L (L = DONOR LIGAND)

Chlorine-35 and 121,123Sb n.q.r. frequencies and their temperature dependencies for various octahedral complexes of antimony pentachloride, SbCl5L (L = donor ligand), are reported. Assignments of 35Cl resonances to axial or equatorial chlorine atoms of the SbCl5 fragment have been possible in some cases. There are no apparent systematic differences between the frequencies of the axial or equatorial chlorine atoms, such differences as there are being masked by crystal-field effects of similar magnitude.

Nuclear quadrupole resonance and stereochemistry. Part 7. The axial and equatorial chlorine atoms in octahedral complexes of antimony pentachloride, SbCl5L (L = donor ligand)

Chlorine-35 and 121,123Sb n.q.r. frequencies and their temperature dependencies for various octahedral complexes of antimony pentachloride, SbCl5L (L = donor ligand), are reported. Assignments of 35Cl resonances to axial or equatorial chlorine atoms of the SbCl5 fragment have been possible in some cases. There are no apparent systematic differences between the frequencies of the axial or equatorial chlorine atoms, such differences as there are being masked by crystal-field effects of similar magnitude.

Complexes of antimony pentachloride with some 4-substituted pyridine N-oxides

The complexes SbCl 5·L (where L = 4-methoxypyridine N-oxide, 4-chloropyridine N-oxide, 4-cyanopyridine N-oxide, 4-nitropyridine N-oxide and 3-ethyl carboxilatepyridine N-oxide) have been isolated and investigated by conductivity, UV and IR spectral measurements. The IR spectra in the range 600–250 cm −1 are consistent with a C 4u symmetry. The NO stretching vibration was insensitive to the substituent variations in the complexes with 4-Z-pyO ligands (where Z = CH 3O, CH 3, H, Cl, CN, NO 2). There is no linear correlation between the Sb-O stretching modes and the σ PyO parameters. A better correlation of the latter with the ππ* ligand band position was found.

Investigation of SbCl5-donor complexes with charge transfer by the NQR method

1. The NQR-121Sb and123Sb spectra of two complexes and35Cl spectra of six complexes of antimony pentachloride were investigated. 2. The degree of charge transfer and the distribution of charge in the acceptor molecule was calculated according to the Daily-Townes theory. 3. The influence of electronic and steric factors on the NQR-35Cl spectra was investigated.

Mössbauer spectroscopy of 121Sb in adduct complexes of antimony pentachloride

The Mössbauer spectra of Sb121 in a variety of oxygen and nitrogen adduct complexes of antimony pentachloride (SbCl5L where L = NCCH3, NCC(CH3)3, NCCl, NCCCl3, OPCl3, OP(Ph)3, DMF, DMSO, NO2CH3, ON(CH3)3, Cl−, Br−) are reported. The experimental data are analyzed using the transmission integral. This technique is shown to be essential in order to get reliable hyperfine interaction parameters. Under these conditions the quadrupole interactions deduced from the Mössbauer spectra are in perfect agreement with those measured by NQR spectroscopy. The dependence of the quadrupole interaction and isomer shift on the donor power of the adduct ligand is explained in terms of the variation of the number of electrons transferred between the antimony atom and the six surrounding ligands and is supported by the NQR data available on the chlorine ions.