Zr-MCM-41的合成及其表征

以Zr(NO3)4·3H2O为锆源，通过直接合成法得到了Zr-MCM-41介孔材料，考察了不同Zr/Si摩尔比对样品的影响，其中Zr/Si的摩尔比最大为0.25。随着Zr/Si的摩尔比的增加，2θ=2°附近的100晶面的衍射峰强度逐渐降低，当Zr/Si摩尔比大于0.25后得不到介孔Zr-MCM-41材料。对所得样品采用XRD、TG-DTA、N2吸附 脱附几种分析方法进行了表征。     

辅酶Q10的合成

以2,3,4,5-四甲氧基甲苯为原料, 经溴化、生成格氏试剂后在碘化亚铜存在下与(E)-4-氯-2-甲基-1-苯磺酰基-2-丁烯缩合得到合成辅酶Q10的关键中间体6-(E-3'-甲基-4'-苯磺酰基-2'-丁烯基)-2,3,4,5-四甲氧基甲苯. 此中间体与茄尼基溴缩合、脱砜基化反应和氧化三步反应, 最终制得标题化合物辅酶Q10, 以2,3,4,5-四甲氧基甲苯计总收率达31.3%.     

Cobalt(II) Chloride Complex Formation in Acetamide–Calcium Nitrate Tetrahydrate Melts

The absorption spectra of Co(II) chloride complexes, containing variable concentrations of chloride ligand, in a molten mixture of 80 mol% acetamide–20 mol% calcium nitrate tetrahydrate, were studied at 313, 333, 353, and 363 K, in the wavelength range 400-800 nm. The melt contains three possible ligands (CH₃CONH₂, H₂O, and NO₃ ^-) for competition with added chloride ligand. Addition of chloride caused a shift of the absorption maximum of octahedral cobalt(II) nitrate towards lower energies and pronounced changes in the shape of the initial spectrum of cobalt(II) nitrate. The effect of temperature changes on the molar absorption coefficient of the Co(II) species was dependent on the chloride concentration and was attributed to the structural changes occurring in the cobalt(II) species. The STAR and STAR FA programs were applied to identify the complex ionic species and to calculate the stability constants of Co(II) complexes formed in this solvent. The results indicate the highest probability of formation of the following complex species: Co(NO₃)₄ ^2-, Co(NO₃)₂Cl₂ ^2-, and CoCl₄ ^2-. Stability constants of each complex were presented for the equilibria occurring at 313, 333, 353, and 363 K. Distribution of the Co(II) species was also calculated over the ranges of chloride concentration and temperature investigated.     

Ln(Ⅲ)与2-羟基-1-萘醛缩蛋氨酸盐及邻菲咯啉三元配合物的合成与表征

合成了稀土硝酸盐与希夫碱盐2-羟基-1-萘醛缩蛋氨酸钾(以KL表示)及邻菲咯啉(Phen)的四种固体三元配合物。通过元素分析，IR，UV，DTA-TG及摩尔电导分析等手段确定配合物的组成为[Ln(L)(Phen)(NO3)(H2O)]NO3(Ln＝Gd，Dy，Er，Yb)，并对它们的配合方式及某些物理和化学性质进行了研究。     

The ternary system H2O–Fe(NO3)3–Co(NO3)2 isotherms 0 and 15 °C

The solid–liquid equilibria of the ternary system H₂O–Fe(NO₃)₃–Co(NO₃)₂ were studied by using a synthetic method based on conductivity measurements.

Two isotherms were established at 0 and 15 °C, and the stable solid phases which appear are the iron nitrate nonahydrate (Fe(NO₃)₃·9H₂O), the iron nitrate hexahydrate (Fe(NO₃)₃·6H₂O), the cobalt nitrate hexahydrate (Co(NO₃)₂·6H₂O) and the cobalt nitrate trihydrate (Co(NO₃)₂·3H₂O).     

[Ce(NO3)5H2O]·(C3H5N2)2的合成、晶体结构及热分析

Colorless crystal, [Ce(NO₃)₅H₂O]·(C₃N₂H₅)₂, has been obtained from the reaction of Ce(NO₃)₃ with imdazole in the aqueous solution and its crystal structure has been determined by single crystal X-ray diffraction techniques.The crystal belongs to triclinic, space group P1. The cell parameters are: a = 0.7489(1) um, b = 0.7914(2) nm, c = 1.8139(3) nm, a = 89.39(2)°, β = 89.37(l) °,γ = 63.18(2)°, Dc = 2.1g·cm^-3, Z = 2, R = 0.0319.In the compound, all of five nitrates are bidentate and one molecule of water is monodentate, the coordination number of Ce (Ⅲ) is 11.The processes of thermal decomposition of the compound was proposed by its TGcurve.     

Etude de l’isotherme 25°C du système quasi quaternaire H2O-Zn(NO3)2·6H2O-Cu(NO3)2·3H2O-NH4NO3;I- Isoplèthes 4 masse% NH4NO3, 8 ma

The solid-liquid equilibria of the quasi-quaternary system H₂O-Zn(NO₃)₂·6H₂O-Cu(NO₃)₂·3H₂O-NH₄NO₃ were studied at 25°C by using a synthetic method based on conductivity measurements. Three isoplethic sections has been established at 25°C and the stable solid phases which appear are: NH₄NO₃(IV), Zn(NO₃)₂·6H₂O, anhydrous Cu(NO₃)₂, Cu(NO₃)₂·3H₂O and metastable Cu(NO₃)·2.5H₂O. Neither double salts, nor mixed crystals are observed at these temperatures and composition range.     

Water in melts: Raman spectral investigation of the molten Ca(NO3)2·4H2O−KNO3 system

The Raman spectra of molten mixtures of Ca(NO₃)₂\4H₂O–KNO₃ have been examined, covering the concentration range of 0–70 mole% KNO₃. The frequencies in the spectra of the mixtures have been found to change slightly with concentration. Striking variations in the band shapes have been observed in the regions corresponding to the O–H stretching mode (2850–3850 cm^–1) and the v₄-NO ₃ ^– mode (700–750 cm^–). The results are discussed in terms of perturbed quasi-lattice structure for the melt, in which there could be a displacement of water molecules in the first coordination sphere around Ca²⁺ by the NO ₃ ^– ion.     

A facile procedure for the one-pot synthesis of unsymmetrical 2,5-disubstituted 1,3,4-oxadiazoles

Unsymmetrically 2,5-disubstituted 1,3,4-oxadiazoles were efficiently synthesized from the cyclization-oxidation reaction of acyl hydrazones. Also, the synthesis of the title compounds was achieved by the condensation of acyl hydrazides and aromatic aldehydes in the presence of ceric ammonium nitrate in dichloromethane.