Abstract:4-(2,2-diphenylethenyl)-N,N-bis[(4-methyl)phenyl] aniline was synthesized with bromodiphenylmethane and 4-(N,N-bis-4-methylphenyl) aminobenzaldehyde via Wittig-Horner reaction. The relationship between yield and reaction conditions, such as reaction time, temperature and the molar ratios of raw material was investigated and the yield could reach 97.94%. The 10 times amplification synthesis were conducted under the above conditions and got the average yield of 96.79%. The compound was characterized by 1H NMR, 13C NMR, FT-IR and MS. The highest occupied molecular orbital (HOMO) level and the lowest unoccupied molecular orbital (LUMO) of the compound were investigated by the cyclic voltammetry experiment, respectively. The organic photoconductive devices based on the titled compound as hole-transporting materials showed excellent xerographic performance, V0 = 550V，VR = 10 V，Rd = 10 V/s, E1/2 = 0.6 lux?s.

Abstract:A novel attapulgite clay -g-poly(2-acrylamido-2-methylpropanesulfonicacid) (APT-g-PAMPS) superabsorbent resin was synthesized by aqueous solution polymerization using microwave irradiation in the presence of Potassium persulfate (KPS) as a initiator and N, N-methylene-bis-acrylamide (MBA) as a crosslinking agent. The chemical structure of APT-g-PAMPS superabsorbent resin was determined by FT-IR and XRD. The influence of the content of APT, microwave power and time on water absorbency was investigated. The swelling behaviors, the water retention and reswelling capability of superabsorbent resin with different APT content were also examined. FITR and XRD characterization indicated that APT and AMPS happened the grafting copolymerization reaction, the reaction occurs only in the APT surface, and AMPS was not inserted into the APT interlayer. Microwave power was 195W, microwave time was 2.5min and APT amount was 5% (mass fraction), the water absorbency of superabsorbent resin in deionized water and normal saline were 987g /g and 102g/g, respectively. The superabsorbent resin has a faster absorption rate, stronger water retention and better reswelling capability. The water absorbency, salt-water performance, water retention and absorption rate of the superabsorbent resin could be remarkably enhanced by introducing a proper amount of APT.

Abstract:Nano silica (SiO2) sol was synthesized through a sol-gel process. Then nano silica sol was modified by KH-570. Polyurethane-acrylate/SiO2 composite latex (SPUA) with core-shell structure was synthesized with modified nano silica, acrylate and polyurethane prepolymer end-capped by double bond by in situ polymerization. The structure of the copolymer was characterized by Fourier transform infrared spectrometer (FTIR). The particle morphology of the SPUA latex was observed through transmission electron microscopy (TEM). Contact angle measuring instrument, tensile testing machine，scanning electron microscopy (SEM) and thermo gravimetric analyzer were performed on the film to test the contact angle to water, mechanical properties, surface appearance and thermal properties of the SPUA films. The results indicated that, with increasing the mass fraction of modified nano silica, the mechanical properties and the thermal stability of the films were improved obviously. When the mass fraction of modified nano silica was 8% in the film,the temperature for the maximal thermal mass-loss rate was 413℃,water absorption was 4.1%, contact angle was 71.5°,the tensile strength of the SPUA film was 17.7MPa and the hardness was 93%.

Abstract:Silver nanoparticles with narrow distribution were prepared by a simple route in water in presence of lauric acid as the capping agents, hydrazine hydrate as reducing agents, silver ammonia as silver source. The morphology and crystal structure of as-synthesised silver nanoparticles were analyzed by transmission electron microscopy and X-ray powder diffraction. The mass ratio of lauric acid and silver nitrate, the reacion temperature pay important roles on the morphology and size of the silver nanoparticles. Well-dispersed silver anopartilces with average diameter of 8 nm were obtained when the mass ratio of lauric acid and silver nitrate was 1.2:1 and the reacion temperature was room temperature. It is also confirmed that the silver particels was monodisperse silver nanoparticles by UV-vis spectra .

Abstract:A lignin model compound composed of α-O-4 and β-5 linkages was synthesized by the radical polymerization with isoeugenol as the raw material and horseradish peroxidase (HRP)/H2O2 as the catalyst. The process variables of the synthesis were investig- ated and the structure of the product was characterized by IR, GC-MS, EA and NMR. It is found that a more than 90% of yield was achieved under the optimal reaction conditions of 1:1 molar ratio of isoeugenol to H2O2, 1.5ml of 10g/L HRP, 3:4 of volume ratio of acetone to phosphate buffer solution, 50℃ of the reaction temperature and 2h reaction time.

Abstract:Friedel-Crafts acylation of salicylaldehyde with bromoacetyl chloride affords 5-(bromoacetyl)-2-hydroxybenzaldehyde(2), which was amination with tert-butylamine and acid hydrolysis, after purification column the intermediate 5-[[(1,1-Dimethylethyl) amino]acetyl]-2- hydroxybenzaldehyde Hydrochloride(3) obtained. The target compound albuterol-D2(4b) was obtained by reduction with boron sodium deuteride. Synthetic routes advantage lies in the last step reaction to introduce deuterium isotope, deuterium labeled isotope abundance was not diluted, and had the advantages of simple operation, short process flow, less side product, The yield was more than 70%. The product was characterized by MS and 1H NMR, the deuterium enrichment was more than 97.1% .

Abstract:The micellization behavior of binary surfactant mixtures containing anionic surfactants with different counter ions viz. sodium dodecyl sulphate (NaDS)and magnesium dodecyl sulphate (Mg(DS)2) and nonionic surfactants with different head group structures viz. n-dodecyl-β-D-maltoside (DDM) and dodecyl tetraethylene glycol ether (Brij30) in aqueous solution were investigated respectively by surface tension and fluorescence probe methods. The results indicated that strong synergistic effect exist between the two components of micelles of all the mixed surfactant systems. The magnitude of synergistic effect followed the order Mg(DS)2/DDM＜NaDS/DDM＜Mg(DS)2/Brij30＜NaDS/Brij30. Mg(DS)2 had less interaction with nonionic surfactants in comparison to NaDS. Mg2+ leaded to MDS in mixed micelle was less far away from the standard state compare with Na+ 。The results of the interaction between surfactants and the contribution of free energy by Maeda’s model were consistent with that of Rubingh’s theory. Moreover, nonionic surfactant with the flexible head group encourages the formation of the mixed micelle and counter ions have little great impact on the aggregation and micropolarity of mixed surfactant systems.

Abstract:A photo-responsive reversible cationic surfactant 4-butylazobenzene-4’-(oxyethyl)trimethylammonium bromide (AZTMA) was synthesized from 4-Butylaniline, 1,2-ethylbromide and phenol by the methods of Williamson ether-forming reaction and amination reaction. The structure of AZTMA was characterized by means of H-NMR, and the results indicated that the product obtained was identical to its theoretical structure. The photo-reversible characteristics of AZTMA were analyzed by full wavelength scanning, and the photoisomerization occurred under the irradiation of ultraviolet light at 360 ±5 nm and visible light at ≥ 420 nm. 50 min is need for trans-AZTMA solution under the irradiation of ultraviolet light to achieve equilibrium, and 90 min for cis-AZTMA under visible light irradiation. The critical micella concentration (CMC) values of trans-AZTMA and cis-AZTMA were detected by adopting the platinum plate method. The CMC of trans-AZTMA was 2.0 mmol/L, while that of cis-AZTMA was 6.0 mmol/L. The results indicated that AZTMA possesses good photo-reversible characteristics and the formation and disintegration of AZTMA micelles can be reversibly controlled.

Abstract:The tyrosine phenol lyase (TPL) from Citrobacter freundii was recombinantly expressed in E. coli BL21 (DE3) with the vector pETDuet-1. The enzymatic properties of recombinant tyrosine phenol lyase were studied, and several influence factors of enzyme reaction such as pH, temperature, surfactants, metal ions, ammonium salts, and ammonium chloride concentration were investigated. The result indicate that the optimum reaction condition of TPL were 45℃, pH 8.0, 4 mmol/l PLP, 350 mmol/l NH4Cl, 1 mmol/l triton-x 100. The conversion rate of pyruvate substrate was 1.8 times higher than that of serine substrate.

Abstract:A gold catalyst Au/meso-?-Al2O3 was synthesized by depositing Au NPs onto a home-made mesoporous ?-Al2O3 via deposition-precipitation method for the CO oxidation. The preparation, drying and calcination conditions were systematically investigated, and the catalysts were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), N2 adsorption isotherm at -196 oC, inductively coupled plasma atomic emission spectrometry (ICP-AES), and Uv-vis DRS. The experimental testing results indicated that the small Au NPs of ~2.0 nm is highly active for the CO oxidation, which could be realized by accurately controlling the preparation, drying and calcination conditions.

Abstract:The polar non-volatiles in the oxidized chicken fat prepared by control oxidation technology were analyzed by solid phase extraction (SPE) combining with liquid chromatography and atmosphere pressure chemical ionization mass spectrometry (LC-APCI-MS) as well as liquid chromatography and electric spray ionization mass spectrometry (LC-ESI-MS). Total of thirty-five kinds of oxidized compounds from glycerides classified as four types including bi-hydroperoxides, mono-hydroperoxides, diacylglycerols and epoxides were identified, among which mono-hydroperoxides (23 kinds) dominated. The mono-hydroperoxides in the oxidized chicken fat were quantified using mono-hydroperoxide of trilinolein as the external standard by LC-APCI-MS. The mono-hydroperoxides in the oxidized chicken fat turned out to be 121.36 mg/kg in total, whereby the mono-hydroperoxides of linoleoyl-dioleoyl-glycerol ranked the highest (45.05 mg/kg). The results indicated that the control oxidation technology was a kind of mild oxidation process, since the oxidized chicken fat was mainly the important flavor precursors of mono-hydroperoxides of triglyceride.

Abstract:Febuxostat was prepared by 4-hydroxybenzonitrile via sulfuration, cyclization, formylation, cyanation, alkylation and hydrolysis. The cyanation and alkylation reaction were performed by one-pot reaction in improved process, and the key factors, such as concentration of hydrochloric acid, reaction time, temperature, the ratio of methane sulfonic acid to trifluoroacetic acid, were explored. The improved process was convenient, mild reaction condition, and the total yield was as high as 65.7%.

Abstract:Based on “Click chemistry”, A series of glycosyltriazole salicylic acid derivatives using glycosyl azide and alkynyl-substituted salicylaldehyde as starting material were synthesized via copper-mediated 1,3-dipolar cycloaddition reactions, oxidation and hydrolysis reaction. The structure was characterized by 1H-NMR, IR, ESI-MS and elemental analysis. These compounds were evaluated for their PTP1B inhibitory activity. The results demonstrated that all compounds presented potent inhibitory activities against PTP1B, among which compounds 4a exhibited most potent with IC50 value of 54.52?0.79μM.

Abstract:The PLA grafted NVP copolymer microspheres were prepared by solvent evaporation extraction method using nimodipine as the model drug and analyzing main factors such as the PLA concentration, the emulsifier concentration, stirring speed and dosing ratio with orthogonal design. The surface morphology of the microspheres was scanned under electron microscope and formulation of microspheres was confirmed by FTIR. Characteristics of the powder partical such as mean diameter, drug loading rate and entrapment rate were evaluated comprehensively, and its in vitro release properties were studied. The results showed the copolymer microspheres were round and the surface was smooth, the average particle size were less than 10μm with narrow particle size distribution, with preparation process of 4% PLA concentration, 3% emulsifier concentration, 9000r/min stirring speed and 2/3 dosing ratio. The microspheres release of more than 14 days, and the release rate increased with the increasing graft ratio.

Abstract:A rapid, accurate and no sample preparation required method was developed by near infared spectroscopy(NIR) to identify 41 (seven categories) solid excipients widly used in pharmaceuatical industry. 6 batches samples in each class were collected and 246 raw NIR spectrograms were obtained. 215 NIR spectrograms were utilised to establish the calibration model and rest 41 spectrograms were utilised to validate the performance of the model. On the original data, second derivative 9 point smoothing combined with the first range of calibration was chosen as the optimum pre-processing method at 3966~10414cm-1, and 30 solid excipients of all the 41 samples could be well identified by this model, namely “model 1”, and the other 5 sublibraries namely models(2-6) were developed for 11 excipients in order to classify every sample sufficiently. With this approach, no “error determinations” were assigned to a wrong class, which indicated the NIR method is appropriate for the identifacation of excipients in the cGMP manufacture of drug products within the pharmaceutical industry.

Abstract:A novel scale and corrosion inhibitor is synthesized by aqueous quadripolymerization with raw materials such as the itaconic acid (IA)，acrylic acid (AA)， 2-acrylamido-2-methy/L-propanesulfonic acid (AMPS) and methyl methacrylate (MMA). Moreover，the preparation procedures of the inhibitor are optimized by the orthogonal experiments. And，95.3 % of scale efficiency for Ca3(PO4)2 ，the transmission rate of iron oxide is 48%，having very good scaling and dispersing capacity， and 75% for CaCO3 could be obtained by evaluating with national standard method when 20 mg/L and 40 mg/L of this quadripolymer is used respecttively，while corrosion efficiency is 74.3%. The analytical results of the infrared spectrum indicate that the quadripolymer contains such ionic groups as the carboxyl ，ester base and sulfonic acid groups.

Abstract:Dimethyl Methylphosphonate(DMMP) and Ethylene Glycol(EG) as raw meterials, p-toluenesulfonic acid(p-TSA) and 1-butyl-3-methylimidazolium tetrafluoroborate ([Bmim]BF4) as synergetic catalysts, a novel polyphosphonate flame retardant was synthesized in a distillation apparatus. The molar ratio of raw meterials, the amount and molar ratio of catalysts and reaction temperature were investigated by L9(33) orthogonal experiment. The optimal synthesis conditions were as follows: the molar ratio of EG to DMMP is 1:1, n([Bmim]BF4)/n(DMMP)=0.01, n(p-TSA)/n(DMMP)=0.02, the reaction temperature at 155-170℃, reaction time at 4h. The synthetic product was yellowish transparent liquid and its acid value was 370 mgKOH/g. The product was characterized by IR and LC-MS analysis and the result showed that the product is a mixer of different polymers. The composition by side reactions which are mainly methanol, dimethyl ether, ethylene glycol monomethyl ether, ethylene glycol dimethyl ether and ethylene glycol reduction were characterized by IR and GC-MS analysis.

Abstract:An acid thickening agent P(AM-DMC-APEG) was synthesized by acrylamide, methacryloxyethyltrimethyl ammonium chloride and allyl polyoxyethylene ether that was with a long chain temperature-sensitive group. The optimal conditions were as follows: monomer concentration 40%, monomer ratio 1:20 :2(APEG:AM:DMC),initiator concentration 0.08%, polymerization temperature 70℃, polymerization time 3.5h. Then molecular structures and molecular weight were characterized respectively by infrared spectrum and static light scattering. After evaluation on temperature sensibility and retarding performance, the results showed that the synthetic P(AM-DMC-APEG) presented good temperature sensibility and retarding performance.

Abstract:The efficient perfluorinated alkyl polyacrylate emulsion (FPE) was synthesized by Tetrahydroperfluorodecylacrylate(FM), Butyl Acrylate(BA), Methyl Methacrylate(MMA)and N, N-Dimethylethanolamine Methacrylate (DM), under the compound emulsifier of octadecyl trimethyl ammonium chloride(1831)and fluorinated emulsifier(FS).This reaction was initiated by potassium persulfate(KPS). The chemical structure and thermostability of emulsion were characterized respectively by IR and Thermogravimetry(TG). The results showed that FM was grafted to the polymer successfully and the decomposition temperature reached to 351.5℃ with the increase of fluorine content. The static water contact angle and atomic force microscope (AFM) were used to test waterproof performance of emulsion. The results showed that when the fluorine content reached to 12%, static water angle would reach to 127°. Particle size analyzer and transmission electron microscope(TEM) were used to detect the microstructure of emulsion. The results show that latex particles are spherical with average size of 220nm and monodisperse.

Abstract:A novel “off-on” rhodamine B schiff fluorescent probe was synthesized by rhodamine B, hydrazine hydrate and Vanillin, it exhibits high selectivity for sensing Cu2 in 50% acetonitrile. The fluorescence titration spectra and the Job's plot indicated the formation of 1:1 complex between 1 and Cu2 , and the complexation process is reversible. For Cu(Ⅱ) concentration in the scope of 0～10 μmol/L, it showed a good linear relationship with a correlation of r=0.9972(n=5) and detection limit of 0.48 μmol/L.

Abstract:With green synthetic technology to avoid organic solvents, the aqueous medium is used to the dethiolation of 2-mercaptopyrimidine derivatives via the reduction activity of Raney-Ni. Specifically, the yield effect on the substitution, reaction solvents and temperature was optimized, along with the recycling possibility of Raney Ni and waster water. 4-Amino-6-hydroxypyrimidine, 4-aminopyrimidine, 5,6-diamino-4-hydroxypyrimidine and 4-hydroxypyrimidine were synthesized with the yields of 98%, 74%, 87% and 89%, respectively. The green synthetic process is stirred under reflux for 1-4 h, which can avoid organic solvents for improving the production safety.

Abstract:The stilbene was synthesized via Wittig-Horner reaction in liquid-liquid phase-transfer catalysis (LL-PTC) system in which the NaOH aqueous solution and nonpolar solvent were used as the aqueous phase and the organic solvent, respectively. The effect of various catalysts, the amount of catalyst, the concentration of NaOH, the temperature and the various solvents were investigated. The activity of various aldehydes for Wittig-Horner reaction in LL-PTC system was also investigated. The optimum reaction condition was ascertained as follows: Tetraoctyl Ammonium Bromide（TOAB） as phase transfer catalysis, n(TOAB): n(Phosphonate)=1:10, 50% NaOH aqueous solution, at 45℃ and toluene as solvent. The yield was more than 96% under optimum reaction conditions. Wittig-Horner reaction showed high isolated yield and geometric selectivity (E-isomer) for various aldehydes in LL-PTC system.

Abstract:In this paper, N-isopropyl acrylamide was synthesized by Cope elimination reaction of amine oxide from methyl acrylate and isopropylamine using diethyamine as the protective agents, hydrogen peroxide as oxidant. The oxidation reactions of DEAPAA and the yields of NIPAM were assayed by HPLC. The effect of the amount of hydrogen peroxide, catalyst and reaction temperature on oxidation reactions of DEAPAA was investigated and the influence factors,such as pyrolysis temperature, vacuum and solvent on the yield of NIPAM were analyzed. The results indicated that with sodium tungstate / sodium pyrophosphate as catalyst, double doses of hydrogen peroxide and reacting at 70℃ for 3 hours, the degree of oxidation of DEAPAA were almost 100% and the yields of NIPAM from Cope elimination reaction were 70%-72% by pyrolysis at 90℃in vacuum.

Abstract:Abstract: This experiment used mPEG with the molecular weights of 1200, 2000 and 5000 as raw materials and adopted the Jones reagent oxidation method to produce CmPEG at ambient temperature. Characterized by 1HNMR and IR, the product was proved to be CmPEG. The carboxyl conversion rate was taken as the index to find out that the most proper molar ratio of Cr2O3 and mPEG was 2 to 1. The carboxyl conversion rates of three products with different molecular weights were 99.63%, 99.4% and 98% respectively. This experiment adopted the solid-liquid extraction technique to reprocess these products and taked the appearance and color as indices. The result shows that the product is produced to be white and of high purity in the order of distilling acetone first and adding sodium bicarbonate to neutralize them next. Taking the yield of these products as the index, used mPEG with the molecular weights of 1000,1200, 2000 ,5000 and PEG with the molecular weights of 800 as raw materials, the experiment shows that this method applies to the preparation of the carboxylic acid derivatives of PEG which molecular weight is more than 2000 and mPEG which molecular weight is more than 1000. The yield of these five products with different molecular weights are 88.2%,93.5%,98.0%,98.2%,39.1% respectively. key word: Methoxypolyethylene glycols; Carboxyl-mPEG; Jones reagent; Cr2O3

Abstract:The synthesis of 3-(N-ethyl-N-methoxycarbonylmethyl)amino acetanilide was reported by 3-aminoacetanilide as starting material via two step reactions. The desired product was yield by the ethylated compound (from 3-aminoacetanilide reacted with acetaldehyde) reacted with methyl chloroacetate. The optimized reaction conditions were as follows: In the first step, The yield of 3-(N-ethyl)amino acetanilide was 90.7% and its purity was up to 97.5%, when the molar rate of acetaldehyde to 3-aminoacetanilide was 1.2 and 5% Pd/C as catalyst under 3.5MPa of hydrogen atmosphere at 70℃. In the second step, the desired product was obtained in 94.6% yield and 96.8% purity with 0.6 equiv. of sodium carbonate as deacid reagent under 70 ℃.