Spectroscopic study on the complex formation of chromogenic bridged calixarenes with aliphatic amines

The complex formation between chromogenic capped calix 4 arene derivatives comprising indophenol indicator group(s), and aliphatic amines has been studied by UV/Vis spectroscopy. The equilibrium constants have been determined in ethanol, and—for one ligand—also in dimethylsulfoxide. The results have been interpreted in terms of various types of host–guest interactions and of steric effects.     

铜、锌在5-Br-PADAP和表面活性剂体系中的分光光度法同时测定

5一Br—PADAP在阳离子表面活性剂溴代十六烷基三甲胺存在下同时测定Cu^2 和Zn^2 ，找出最佳实验条件，对水和血清测定结果令人满意．     

The influence of hard‐segments on two‐phase structure and shape memory properties of PCL‐based segmented polyurethanes

Poly(ε‐caprolactone)‐based segmented polyurethanes (PCLUs) were prepared from poly(ε‐caprolactone) diol, diisocyanates (DI), and 1,4‐butanediol. The DIs used were 4,4′‐diphenylmethane diisocyanate (MDI), 2,4‐toluenediisocyanate (TDI), isophorone diisocyanate (IPDI), and hexamethylene diisocyanate (HDI). Differential scanning calorimetry, small‐angle X‐ray scattering, and dynamic mechanical analysis were employed to characterize the two‐phase structures of all PCLUs. It was found that HDI‐ and MDI‐based PCLUs had higher degree of microphase separation than did IPDI‐ and TDI‐based PCLUs, which was primarily due to the crystallization of HDI‐ and MDI‐based hard‐segments. As a result, the HDI‐based PCLU exhibited the highest recovery force up to 6 MPa and slowest stress relaxation with increasing temperature. Besides, it was found that the partial damage in hard‐segment domains during the sample deformation was responsible for the incomplete shape‐recovery of PCLUs after the first deformation, but the damage did not develop during the subsequent deformation. © 2007 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 557–570, 2007     

Liquid Chromatography-Mass Spectrometry Determination of Six 5-Nitroimidazoles in Animal Feedstuff

A liquid chromatography-mass spectrometry method for the determination of the coccidiostats metronidazole, ronidazole, dimetridazole, secnidazole, tinidazole and ipronidazole in feedstuff was developed. The 5-nitroimidazoles were extracted from animal feed with a pH 2 phosphate buffer solution followed by a solid phase extraction procedure based on HLB cartridges. The liquid chromatographic separation of the extracts was performed on a C₁₈ bonded silica column applying a gradient of elution with pH 4.3 ammonium acetate buffer solution and acetonitrile. Quantification for each 5-nitroimidazole was carried out monitoring its molecular ion [M + H]⁺ obtained by positive electrospray ionisation mode. A pool of feedstuffs was used to optimise and validate the method. Linearity, quantification limit, intra-day and inter-day reproducibility and accuracy were estimated using this pool of feedstuffs spiked with the drugs. For the confirmatory assay, several fragment ions from each 5-nitroimidazole were obtained and monitored. The method was applied successfully to determine 5-nitroimidazoles in feedstuff at level of 0.05 mg kg⁻¹.     

An unusual 1,2-N→C acyl migration in urea derivatives of α-aminoorganolithiums

Transmetalation of urea derivatives of α-aminoorganostannanes with alkyllithiums provides α-aminoorganolithiums which undergo rapid N to C acyl migration to afford α-aminocarboxamides. The stereochemical course of the transmetalation/migration process depends on the substituents on the urea and varies from complete retention of configuration to complete racemization.     

Synthesis and properties of tricyclo[6.4.1.0]trideca-1,3(6),7,9,11-pentaene

A new cyclobutene-fused 1,6-methano[10]annulene was synthesized by pyrolysis of the sulfone and sulfinate adducts of 3,4-bis(methylene)-1,6-methano[10]annulene and its physical and chemical properties were disclosed.     

Formation of 2,6-dioxabicyclo[3.3.0]-octa-3,7-dienes or multiply substituted o-benzoquinones from reactions of 1,4-dilithio-1,3-dienes with dimethyl oxalate

Reactions of 1,4-dilithio-1,3-dienes with dimethyl oxalates afforded multiply substituted o-benzoquinones or stereodefined 2,6-dioxabicyclo[3.3.0]-octa-3,7-dienes in good yields.     

Synthesis of Methyl 2-(5-Arylidene-2,4-dioxotetrahydrothiazol-3-yl)propionates

A series of methyl 2-(arylidene-2,4-dioxotetrahydrothiazol-3-yl)propionates were prepared. A study of the 3D structure was performed. The log P values are given for all the synthesized compounds.     

Crystallographic report: Crystal structure of tetra(4‐methyl‐5‐imidazole‐carboxyaldehyde)zinc(II) diperchlorate

The central zinc(II) atom in the title complex is tetrahedrally coordinated by four nitrogen atoms derived from 4‐methyl‐5‐imidazolecarboxyaldehyde ligands with Zn? N in the range 2.007(3) to 2.026(4) Å. Copyright © 2003 John Wiley & Sons, Ltd.     

New 6-Arylsulfonyl-1,2-benzoisothiazol-3(2H)-one 1,1-Dioxides Derived from Diphenyl Sulfone Monosulfonyl Chlorides

Various methods were studied for the oxidation of 2-methyl-5-(phenylsulfonyl)benzenesulfamide and its derivatives. The oxidation by sodium dichromate in sulfuric acid was found most efficient. The effects of temperature, concentration, reagent ratio, and time of the oxidation reaction on the yield of the desired product were investigated. Conditions were proposed for obtaining the desired product in yields up to 95%. A synthesis was developed for a series of new saccharin derivatives.