SYNTHESIS AND PROPERTIES OF POLY(ANILINE-CO-ANISIDINE)

Aniline and ortho-anisidine were chemically copolymerized at various temperatures and monomer compositions. Copolymers completely soluble in THF are prepared and characterized.

STUDIES ON OLEFIN-COORDINATING TRANSITION-METAL CARBENE COMPLEXES .20. SYNTHESIS OF 1,3-CYCLOHEXADIENE(DICARBONYL) [ETHOXY(ARYL)-CARBENE]IRON COMPLEXES AND THEIR PHOSPHINE ADDUCTS - CRYSTAL-STRUCTURE OF C6H8(CO)2FEC(OC2H5)C6H4CH3-O

Reaction of 1,3-cyclohexadiene(tricarbonyl)iron (1) with ortho-substituted aryllithium reagents ArLi (Ar=o-CH3C6H4, o-CH3OC6H4, o-CF3C6H4) in ether at low temperature, and subsequent alkylation of the acylmetalates formed with Et3OBF4 in aqueous solution at 0-degrees-C or in CH2Cl2 at -60-degrees-C gave the 1,3-cyclohexadiene(dicarbonyl)[ethoxy(aryl)carbene]iron complexes (eta4-C6H8)(CO)2FeC(OC2H5)Ar (3, Ar = o-CH3C6H4; 4, Ar = o-CH3OC6H4), and the isomerized product (eta3-C6H8)(CO)2FeC(OC2H5)C6H4CF3-o (5), respectively, among which the structure of 3 has been established by an X-ray diffraction study. Complex 3 is monoclinic, space group P2(1) with a = 8.118(4), b = 7.367(4), c = 14.002(6) angstrom, beta = 104.09(3)-degrees, V = 812.2(6) angstrom3, Z = 2, D(c) = 1.39 g cm-3, R = 0.056, and R(w) = 0.062 for 976 observed reflections. Complexes 3 and 5 were converted into the chelated allyliron phosphine adducts(eta3-C6H8)(CO)2(PR31)FeC(OC2H5)Ar (6, Ar = o-CH3C6H4, R1 = Ph; 7, Ar = o-CH3C6H4, R1 = OPh; 9, Ar = o-CF3C6H4, R1 = Ph), by reaction with phosphines in petroleum ether at low temperatures.

Synthesis of NiWO4 nano-particles in low-temperature molten salt medium

Nickel tungstate (NiWO4) nano-particles were successfully synthesized at low temperatures by a molten salt method, and characterized by Xray diffraction (XRD), transmission electron microscopy (TEM) and ultraviolet visible spectra techniques (UV-vis), respectively. The effects of calcining temperature and salt quantity on the crystallization and development of NiWO4 crystallites were studied. Experimental results showed that the well-crystallized NiWO4 nano-particles with about 30 nm in diameter could be prepared at 270 degrees C with 6:1 mass ratio of the salt to NiWO4 precursor. XRD analysis confirmed that the product was a pure monoclinic phase of NiWO4 with wolframite structure. UV-vis spectrum revealed that NiWO4 nano-particles had good light absorption properties in both ultraviolet and visible light region. (C) 2009 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Synthesis of nanometric-size magnesium nitride by the nitriding of pre-activated magnesium powder

Magnesium nitride (Mg3N2) was synthesized by the reaction of magnesium in the highly reactive form (Mg*) with nitrogen at 450 degrees C under normal pressure. The effect of doping with nickel dichloride on the nitridation of Mg* was investigated. Differential thermal analysis (DTA) of Mg* systems and transmission electron microscopy (TEM) measurement of the product formed were carried out. TEM measurement showed that the particle size of the Mg3N2 synthesized was in the nanometric range. The dependence of nitridation of the NiCl2-doped Mg* on temperature was investigated at temperatures ranging from 300 to 500 degrees C. The nitridation of NiCl2-doped Mg* could occur even at temperature as low as 300 degrees C. (C) 1999 Kluwer Academic Publishers.