Synthesis and characterization of six-arm star-shaped liquid crystalline cyclotriphosphazenes

<正>The synthesis and mesomorphic properties of a new class of liquid crystalline cyclotriphosphazenes with rigid cyanostilbene groups and flexible alkoxy groups are reported.The thermal behaviors of cyclotriphosphazene derivatives 5a-5d are studied by the means of differential scanning calorimetry,polarizing optical microscopy.Nematic phases were observed in compounds 5a-5d both on heating and cooling.The clear temperatures of compounds 5a-5d slightly increased with increasing length of terminal alkyl chain.Compounds 5a-5d showed different mesogenic region from minimum 5℃to maximum 142℃.     

A convenient synthesis of pyrroles catalyzed by acidic resin under solvent-free condition

<正>A convenient and effective Paal-Knorr condensations of 2,5-hexanedione with most amines have been carried out at room temperature under solvent-free condition.Macroporous strongly acidic styrol resin(D001) as a novel,efficient,cost-effective,and reusable solid acid catalyst for the synthesis of pyrroles under the same conditions.The pyrroles were obtained in high yields in short reaction times.     

Study on curing reaction of 4-aminophenoxyphthalonitrile/bisphthalonitrile

<正>A series of phthalonitrile blending resins were prepared from 4-aminophenoxyphthalonitrile(APN) and 4,4'-bis(3,4- dicyanophenoxy)biphenyl(BPH) by directly powder-mixing and copolymerization.Differential scanning calorimeter(DSC) and dynamic rheology were used to study the curing reaction behaviors of APN/BPH blends,and the results indicated that the introduction of APN accelerated the curing rate of BPH,and the existence of BPH decreased the curing temperature of APN/BPH systems.The thermal stability of postcured APN/BPH resins was investigated by thermogravimetric analysis(TGA),and the TGA results indicated that the crosslinked polymers of APN/BPH systems possessed good thermal stability.     

Electrochemical biosensing for dsDNA damage induced by PbSe quantum dots under UV irradiation

<正>An electrochemical sensor for the detection of the natural double-stranded DNA(dsDNA) damage induced by PbSe quantum dots(QDs) under UV irradiation was developed.The biosensing membranes were prepared by successively assembling 3- mercaptopropionic acid,polycationic poly(diallyldimethyl ammonium) and dsDNA on the surface of the gold electrode.Damage of dsDNA was fulfilled by immersing the sensing membrane electrode in PbSe QDs suspension and illuminating it with an UV lamp. Cyclic voltammetry was utilized to detect dsDNA damage with Co(phen)_3~(3+) as the electroactive probe.The UV irradiation,Pb~(2+) ions liberated from the PbSe QDs under the UV irradiation and the reactive oxygen species(ROS) generated in the presence of the PbSe QDs also under the UV irradiation were the three factors of inducing the dsDNA damage.The synergistic effect of the three factors might dramatically enhance the damage of dsDNA.This electrochemical sensor provided a simple method for detecting DNA damage,and may be used for investigating the DNA damage induced by other QDs.     

Facile synthesis of a melt-spinnable polyborazine from asymmetric alkylaminoborazine

<正>A novel asymmetric alkylaminoborazine monomer,2-propylamino-4,6-bis(methylamino)borazine,was synthesized for the first time,and directly polymerized to give a melt-spinnable polyborazine(PBN).This asymmetric alkylaminoborazine was synthesized by an aminolysis reaction of 2,4,6-trichloroborazine(TCB) with different amines under mild conditions.This route turns out to be much cheaper and simpler than the conventional routes.The chemical composition,structure,molecular weights and ceramic yield were investigated by EA,FTIR,NMR,GPC and TG analysis.The PBN exhibits suitable rheological property for melt-spinning, which suggests that it is a potential precursor for BN fibers.     

Investigation of the interaction of carbofuran and DNA by voltammetry and fluorescence with the aid of chemometrics

<正>The interactions of carbofuran and DNA were studied using voltammetry and fluorescence spectroscopy.The formation of carbofuran-DNA makes the current peak of DNA decreased by voltammetry method.The binding number(n) and constant(K_a) for complex carbofuran-DNA were calculated to be 1.06±0.04 and 0.11±0.03mol~(-1) L,respectively by fluorescence measurement.Chemometrics approach,such as singular value decomposition(SVD) was used to evaluate the number of spectral species in the drug-DNA binding process.And the pure spectra and concentration profiles in the kinetic system were clearly deduced by multivariate curve resolution alternating least squares(MCR-ALS) with the initial estimates by evolving factor analysis(EFA).     

Antigens synthesis and antibodies preparation for furazolidone and its metabolite 3-amino-2-oxazolidinone

<正>Two haptens of 3-[(5-amino-furan-2-ylmethylene)amino]oxazolidin-5-one(FZ-NH_2) and 3-{[(4-carboxyphenyl)methylene]-amino} -2-oxazolidinone(CPAOZ) were synthesized.For FZ-NH_2,immunogens were prepared by glutaraldehyde and diazo salt methods.For CPAOZ,immunogens were connected by the methods of the active ester and mixed acid anhydride.Compared with the combination,indirect competitive enzyme-linked immunosorbent assay(ic-ELISA) was developed with coating antigen of FZ-NH_2 -OVA via the glutaraldehyde method and immunogen of CPAOZ-KLH via active ester method.For furazolidone and its metabolite AOZ(NPAOZ as derivative),the sensitivities(IC_(50)) were 2.0μg/L and 2.5μg/L,limits of detection(IC_(15)) were 0.09μg/L and 0.25μg/L,respectively.A sensitive method was developed for the simultaneous determination of furazolidone in feed and its metabolite AOZ in tissue.     

Synthesis and characterization of an intermediary of new heat-resistant energetic materials

<正>Nitration of 4,4'-biphenyldicarboxylic acid(BPDC) was studied and an aromatic carboxylic acid containing two nitro groups was synthesized and characterized through elemental analysis and IR spectra.Crystal structure of DNBPDC(DNBPDC=2,2'- dinitro-4,4'-biphenyldicarboxylic acid) was determined by X-ray single crystal diffraction and the thermal decomposition was carried out through DSC and TG-DTG analyses.     

Protecting-group-free amination of halogenated nitrobenzaldehyde with palladium catalyst

<正>"One-step"method for the synthesis of secondary aliphatic amine substituted nitrobenzaldehyde was developed.In the presence of Pd catalyst,halogenated nitrobenzaldehyde could be smoothly coupled with secondary aliphatic amine to give the target product in hexamethylphosphamide(HMPT) media without the protection of aldehyde groups.     

A simple and efficient method for solvent-free iodination of hydroxylated aromatic aldehydes and ketones using iodine and iodic acid by grinding method

<正>Green,mild and efficient iodination of hydroxylated aromatic aldehydes and ketones using iodine and iodic acid in the solidstate by grinding under solvent-free conditions at room temperature.This method provides several advantages such as environmentally friendly,short reaction times,high yields,non-hazardous and simple work-up procedure.