Synthesis and characterization of laterally substituted bis(alkoxybenzoyloxy)hydroquinones

A new series of laterally substituted bis(alkoxybenzoyloxy)hydroquinone compounds has been synthesized and their mesomorphic properties studied. A number of hydroquinone compounds were synthesized with terminal n -alkoxy chains ranging from n -butyloxy to n -decyloxy. Additionally, lateral substituents ranging from n -butyl to n -octyl were incorporated through esterification at the remaining unsubstituted phenolic oxygen atoms. By optimizing the combination of the end group and lateral moieties we were able to tailor the molecular structure to form different liquid crystalline phases.     

Synthesis of substituted bis(heteroaryl)maleimides

Substituted bis(fur-2-yl), bis(fur-3-yl) and bis(thien-2-yl) maleimides with potential antidiabetic properties are described. Their synthesis involves, as a key step, a Suzuki cross-coupling between various boron derivatives and the diiodomaleimides. Therefore, a wide range of substituted symmetric and non-symmetric maleimide derivatives can be prepared.     

Synthesis and characterization of bis(cyclopentadienyl)bis(hexafluoroantimonato) titanium(IV)

Reaction of titanocene dichloride with two equivalents of silver hexafluoroantimonate in sulphur dioxide quantitatively yields Cp₂Ti(SbF₆)₂ (Cp = η⁵-C₅H₅) and AgCl. The titanocene bishexafluoroantimonate was recrystallized from SO₂ and characterized by chemical analysis, ¹H NMR, IR and mass spectroscopy.     

Synthesis and characterization of sodium bis(trimethylstannyl) amide and bis(trimethylsilyl) bis(trimethylstannyl) -phospha-tetrazene

Sodium bis(trimethylstannyl)amide NaN(SnMe₃)₂, isolated by the reaction of trimethylstannyldiethylamine with sodium amide, reacts with tris(trimethylsilyl)hydrazino—dichloro-phosphine to form bis(trimethylsilyl)bis(trimethylstannyl)-2-phospha-2-tetrazene, (Me₃Si)₂N-N=P-N(SnMe₃)₂. Both the molecules have been isolated and characterized.     

Synthesis and characterization of copper(II) chelate with a new substituted bis(2-pyridyl)-amine derivative

The novel ligand, abbreviated Ibdpam, has been synthesized and characterized as well as its novel mononuclear copper(II) complex. The crystal and molecular structure of the complex [Cu^II(Ibdpam)(SO₄)(H₂O)₂]·H₂O is reported. The square-based pyramidal arrangement of the chromophore CuN₂O₃, the bidentate chelate character for the nitrogenous base, and the unidentate character of the sulfate oxy-dianion is established.     

Synthesis, characterization and some properties of novel bis(pentafluorophenyl)methoxyl substituted metal free and metallophthalocyanines

The preparation of some new tetrakis[bis(pentafluorophenyl)methoxyl] substituted metal free and metallophthalocyanine (MPcs) complexes were achieved by the tetramerization of 4-[bis(pentafluorophenyl)methoxy]phthalonitrile with Li metal in pentan-1-ol or metal [Co(II) or Zn(II)] acetates in DMAE, respectively. The structures of the target compounds were confirmed by elemental analysis, IR, UV–vis, ¹H NMR, ¹⁹F NMR and mass spectroscopic methods. MPcs are soluble only in strong and medium polar solvents while the metal free one is soluble in weakly, medium and strong polar solvents. The temperature and frequency dependence of the electrical conductivities were studied on spin coated films of the compounds using dc and impedance spectroscopy techniques in the frequency range from 40 to 10⁵ Hz and within the temperature range from 290 to 440 K. The temperature dependence of the exponent s and conductivity, σ_ac, were completely in agreement with the prediction of the hopping model. The redox properties of the complexes were determined by cyclic voltammetry. The nature of the redox processes was also confirmed using spectroelectrochemical measurements.     

Synthesis of laterally substituted bistolane liquid crystals

Methods for synthesizing bistolane liquid crystal materials with lateral methyl and ethyl substituents are presented. Some of the bistolanes are nematic at room temperature. These highly conjugated mesogens exhibit wide nematic ranges, small enthalpies of fusion, high birefringence and modest viscosity. Their potential applications for flat panel displays employing light scattering or Bragg reflection and for infrared optically phased arrays are foreseeable.     

Synthesis of laterally substituted bistolane liquid crystals

Methods for synthesizing bistolane liquid crystal materials with lateral methyl and ethyl substituents are presented. Some of the bistolanes are nematic at room temperature. These highly conjugated mesogens exhibit wide nematic ranges, small enthalpies of fusion, high birefringence and modest viscosity. Their potential applications for flat panel displays employing light scattering or Bragg reflection and for infrared optically phased arrays are foreseeable.     

Synthesis and properties of novel aromatic polyhydrazides and poly(amide–hydrazide)s based on the bis(ether benzoic acid)s from hydroquinone and substituted hydroquinones

4,4′‐(1,4‐Phenylenedioxy)dibenzoic acid as well as the 2‐methyl‐, 2‐tert‐butyl‐, or 2‐phenyl‐substituted derivatives of this dicarboxylic acid were synthesized in two main steps from p‐fluorobenzonitrile and hydroquinone or its methyl‐, tert‐butyl‐, or phenyl‐substituted derivatives. Polyhydrazides and poly(amide–hydrazide)s were prepared from these bis(ether benzoic acid)s or their diacyl chlorides with terephthalic dihydrazide, isophthalic dihydrazide, or p‐aminobenzoyl hydrazide by means of the phosphorylation reaction or low‐temperature solution polycondensation. Most of the hydrazide polymers and copolymers are amorphous and readily soluble in various polar solvents such as N‐methyl‐2‐pyrrolidone (NMP) and dimethyl sulfoxide. They could be solution‐cast into transparent, flexible, and tough films. These polyhydrazides and poly(amide–hydrazide)s had T_gs in the range of 167–237°C and could be thermally cyclodehydrated into the corresponding poly(1,3,4‐oxadiazole)s and poly(amide–1,3,4‐oxadiazole)s approximately in the region of 250–350°C, as evidenced by the DSC thermograms. All the tert‐butyl‐substituted oxadiazole polymers and those derived from isophthalic dihydrazide were organic soluble. The thermally converted oxadiazole polymers exhibited T_gs in the range of 208–243°C and did not show significant weight loss before 450°C either in nitrogen or in air. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 1169–1181, 1999     

相转移催化法合成双3－苯丙烯酰基取代硫脲及双3－苯丙烯酰基取代胺衍生物

以3－苯丙烯酸为原料，经酰氯化，得到3－苯丙烯酰氯，在PEG－400为催化剂 的固液相转移催化条件下与硫氰酸铵及二胺类反应，一锅法制得双3－苯丙烯酰基 取代硫脲化合物。3－苯丙烯酰氯在PEG－600为催化剂的液液相转移催化条件下和 二胺类反应得到双－苯丙烯酰基取代胺化合物。反应条件温和、产率高。化合物经 元素分析、IR及^1H NMR证实。初步的生理活性研究表明，部分化合物具有良好的 抗炎活性。     

Synthesis and properties of some laterally substituted liquid crystals

This paper presents a number of laterally substituted liquid crystalline compounds which have been synthesized by systematically varying both the position and the type of the lateral substituent. The influences of such structural changes on the physico-chemical properties of new compounds are discussed and compared with those of the corresponding laterally unsubstituted analogues.     

Synthesis and characterization of bis(dicarboxylato)dimolybdenum(II) compounds

The reaction of tetrakis(μ-acetato)dimolybdenum(II) in aqueous suspension with various dicarboxylic acids yields compounds of the general formula, Mo₂(dicarboxylate)₂·nH₂O. Phthalic acid also gives tri- and tetra-phthalates, and 1,8-naphthalene dicarboxylic acid yields only the tris complex. For malonic and acetylenedicarboxylic acids, only partial substitution occurs. Tetrakis(μ-acetato)dimolybdenum(II) in aqueous suspension also reacts with monocarboxylic acids, and with benzoic acid, Mo₂(benzoate)₄ is obtained. A polymeric structure is suggested for these compounds in the light of their spectral properties.     

Synthesis and characterization of mono- and bis(pentafluorosulfur)diacetylene

The synthesis of novel, high density, diacetylene monomers has been achieved by the preparation of mono- and bis(pentafluorosulfur) diacetylene. The derivatives are readily prepared by the addition of pentafluorosulfur bromide (SF₅Br) to diacetylene (C₄H₂) and subsequent dehydrobromination. Details of the synthesis and properties of these compounds are discussed.     

Synthesis and characterization of a silyl substituted bis(indenyl) zirconium dichloride and comparison of its olefin polymerization behavior to a siloxy substituted analogue

The synthesis and characterization of rac‐[ethylenebis(1‐(tert‐butyldimethylsilyl)‐3‐indenyl)]zirconium dichloride ( 3 ) is reported. The silyl substituted 3 /MAO was compared to its siloxy substituted analogue ( 4 ) in ethylene homo‐ and in ethylene‐1‐hexene copolymerizations to elucidate the effect of the heteroatom on polymerization performance. The influence of monomer and cocatalyst concentration and the polymerization temperature was investigated. The oxygen between the indenyl ligand and the bulky tert‐butyldimethylsilyl group in the siloxy substituted 4 /MAO was found to have a positive influence on polymerization activity and copolymerization performance. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 39: 127–133, 2001     

Synthesis and characterization of polyesters from hindered biphenols and hydroquinones

Polyesters have been synthesized by polycondensation of terephthaloyl dichloride or isophthaloyl dichloride with hindered biphenols and hydroquinones which contain bulky substituents (methyl and phenyl) on the arylene ring. Polymers derived from isophthaloyl dichloride have better solubility and lower glass transition temperatures than the corresponding polymers obtained from terephthaloyl dichloride. © 1994 John Wiley & Sons, Inc.     

Synthesis and characterization of bis(di-2-pyridylmethanamine)ruthenium(II)

The complex Ru(dipa)(2)(2+) (dipa = di-2-pyridylmethanamine) has been prepared, yielding approximately a statistical ratio of the meso and rac isomers. The electronic spectra of both isomers show pyridyl pi --> pi transitions in the UV region and MLCT bands in the visible region. The solvent dependence of the spectra provides evidence of hydrogen bond formation between the solvent and the NH(2) site on the ligand. The electrochemical properties of the two isomers are identical; each undergoes a reversible one-electron oxidation in acetonitrile (E(1/2) = 0.933 V vs Ag/AgCl) and in aqueous solution below pH 3 (E(1/2) = 0.786 V vs Ag/AgCl). In aqueous solution above pH 3, one-electron oxidation of the ruthenium center is followed by deprotonation of the ligand NH(2) site yielding a reactive amidoruthenium(III) species. The ruthenium-bound dipa ligand possesses structural constraints that prevent the usual oxidative dehydrogenation reaction, which would yield exclusively the corresponding imine. Instead the amidoruthenium(III) intermediate finds alternative reaction routes leading to multiple products.     

Synthesis and characterization of nickel(II) bis(alkylthio)salen complexes

NiX2(2-RSC6H4CH=NCH2CH2N=CHC6H4SR-2) (NiX2L; L = 5) (1a, X = Br, R = C6H13; 1b, X = Cl, R = C12H25) and NiX2(2-C6H13SC6H4CH2NHCH2CH2NHCH2C6H4SC6H13-2) (NiX2L; L = 6) (2a, X = Br; 2b, X = Cl; 2c, X = OClO3) were prepared from ligands 5 and 6, respectively. The 1:2 metal-ligand complex Ni(OClO3)2(2-RSC6H4CH2NHCH2CH2NHCH2C6H4SR-2)2 3, was obtained from an EtOH solution of 2c. The characterization of paramagnetic 1-3 included single-crystal X-ray diffraction studies of 1a and 3. Complex 2c converted into 3 in the presence of excess ligand 6 in CHCl3.