A Novel Green Preparation of a, a''''-Bis (substituted benzylidene)-cycloalkanones Promoted by FeCl_3 6H-2O in Ionic Liquid

a, a'-Bis(substituted benzylidene)cycloalkanones were efficiently prepared from cycloalkanones and benzaldehydes in [bmim][BF4] by using iron(III) chloride hexahydrate as a catalyst. It is shown that [bmim][BF4] and iron(III) chloride hexahydrate can be quantitatively recovered and be reused effectively for many times. Compared with the known methods, this novel process has the advantage of being an envkonmentally benign process together with good yields and mild reaction conditions.     

2-苯甲酰基-N-芳基氨基脲的合成及抑菌活性

以N-取代三氯乙酰胺在碱催化下与苯甲酰肼反应,合成了8种2-苯甲酰基-N-芳基氨基脲3a～3h,其结构经元素分析、IR和1H NMR所表征;初步生物活性测定表明,部分化合物对大肠杆菌、枯草杆菌和金黄色葡萄球菌具有一定的抑菌活性.     

Dimerization of some substituted benzoic acids in aqueous solution from conductance measurements

Precision molar conductances of benzoic, o-toluic, 2,6-dimethylbenzoic, 2,3,6-trimethylbenzoic, and, o-fluorobenzoic acids have been determined in aqueous solution as a function of temperature and of concentration up to near saturation (<0.035 M). At the higher concentrations molar conductances are found to be less than anticipated for the simple dissociation of a 1-1 electrolyte. Although the deviations are only 1% or less they have been interpreted to show that these acids are dimerized in solution. The interpretation includes an assumption that the dimer ionizes to produce a triple ion. Increasing numbers of methyl groups lead to increasing dimerization. For those acids with two ortho groups the dimerization increases with increasing temperature while the other three show decreasing dimerization with increasing temperature. Temperature functions have been determined for the dimerization constants and from these functions standard changes in enthalpy, entropy, and heat capacity have been determined. Comparisons are made with dimerization studies in non-aqueous solvents. From these as well as the behavior of benzene in water it is concluded that a major factor driving the dimerization is hydrophobic interaction. To provide a limiting conductance of the triple ion needed in the dimerization calculations a conductance study was also made for o-Phenylbenzoic acid on the assumption that its anion provides an approximate model of the triple ion.     

2-(1,11-十一亚甲基)-5-取代亚氨基-△~3-1,3,4-噻二唑啉的合成及杀菌活性

通过环十二酮与 N -取代氨基硫脲的缩合反应 ,合成了一系列 N -取代环十二酮缩氨基硫脲 ,经Mn O2 氧化关环 ,得到 1 5种未见文献报道的标题化合物 ,其结构经 IR,1 3C NMR,元素分析的确证 .初步实验表明 ,部分化合物具有一定的杀菌活性     

Construction of solid-liquid phase diagrams in ternary systems by titration calorimetry

Titration calorimetry was used to construct the solid-liquid equilibrium line in ternary systems containing the solute and an aqueous mixed solvent by measuring the heat of dissolution of the solid solute during successive additions of the liquid solvent. The plot of cumulated heats versus the mole ratio, n_solvent/n_solute, yields two (almost) linear increases of different slopes. These two lines represent successively the enthalpy of dissolution then the enthalpy of dilution of the medium; their intersection gives the solubility and the enthalpy of dissolution of the solute. Phase diagrams have been established over the whole concentration range for o-anisaldehyde, 1,3,5-trimethoxybenzene and vanillin, in water + methanol, +ethanol, or +n-propanol at 303, 313 and 318 K.     

离子液体中用Heck反应合成2-取代萘烯丙醇化合物

利用Heck反应, 在离子液体、金属钯或镍、碱和膦配体反应体系中, 由卤代萘与烯丙醇反应, 制得了高收率和高选择性的2-取代萘烯丙醇化合物. 该方法原料便宜易得、操作简单、反应体系可循环使用. 并讨论了醋酸镍替代醋酸钯、不同膦配体、溶剂及碱对反应转化率的影响. 通过核磁共振、红外光谱、质谱和元素分析对产物的结构进行了表征.     

Wittig-Olefinierung zu neuen donor- und akzeptor-substituierten 3-Vinylindolen: Optimierte Syntheseverfahren

Summary The optimized Wittig reaction of selectively functionalized 3-acylindoles yield new, and for Diels-Alder reactions highly reactive donor- and acceptor substituted 3-vinylindoles, respectively.

     

Synthesis and properties of substituted 2-methylene-hydrazono-2,3-dihydro-3-benzo[<Emphasis Type="Italic">b</Emphasis>]furanones

The reaction of 2,3-dihydro-2,3-benzo[b]furandione with the triphenylphosphazines of diazo compounds leads to substituted 2-methylenehydrazono-2,3-dihydro-3-benzo[b]furanones, which are hydrolyzed in an acidic medium to the substituted methylenehydrazides of o-hydroxyphenylglyoxalic acid and react with amines to form the products of addition at the activated CH=N bond of the side chain or 2-hydrazono-2,3-dihydro-3-benzo[b]furanone respectively. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 817–822, June, 2007.     

取代乙酸配体对乙炔二聚反应催化剂性能的影响

研究了取代乙酸配体作为Ｎｉｅｕｌａｎ催化剂对乙炔二聚反应性能的影响。结果表明，不同功能结构数目的影响，结果表明，不同功能结构数目的的氨羧配体均使催化剂的选择性提高。乙炔转化率略有下降，巯基乙酸配体的加入，则改变了乙炔二聚反应的机理，得到以乙醛为主的产物。