Abstract:The first analogue of Trichodermamide T-1 was synthesized from 3-ethoxycarbonyl-8a- methoxy-4,4a,5,8-tetrahydro-1,2-benzoxazine (1a) in 61.6% by hydrolysis in alkaline alcohol solution and amidation reaction with amino-coumarin(2), subsequently. The structure of the compound T-1 was determined by 1HNMR, 13C-NMR，IR and elemental analysis. Investigation on the hydrolysis reaction showed that the bicyclic oxazine ester (1a) can be converted to the oxazine acid (1c) by losing the –OCH3 group. However, the double oxygen-bearing carbon structure of 8a on the oxazine ring can keep stable in the same condition.

Abstract:Abstract: A series of mesoporous strontium-doped titania (Sr-TiO2) materials were synthesized by solid-phase route. These materials were characterized using XRD, TEM, UV-Vis, BET, Raman measurement techniques; their photocatalytic activities were evaluated by measuring the photodegradation of O-nitrophenol solution under UV irradiation. The results showed that the crystal lattice of Sr-TiO2 was anatase phase, the special surface area of a typical product was 160.9m2/g, and pore size distribution was 7.2 nm. Because of Strontium doping, there was slight distortion in the crystal structure of TiO2, and Red-Shift can be seen on absorption band; Under UV irradiation, the photodegradation performance of Sr-TiO2 was improved obviously compared with that of pure TiO2, reached 98.2% in 2 hours. The photocatalytic efficiency reached the maximum when the initial concentration Of O-nitrophenol solution was 30 mg/L and catalyst amount was 1.2g/L.

Abstract:The preparation of PANI/PAA composite films was carried out by the direct polymerization method and the layer by layer method. The surface structure and the composition of the composite films were characterized by scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FT-IR); the cyclic voltammetry (CV), the current response characterization (CA) and the electrochromic characterization were also mensurated. It was found that SEM and FT-IR results showed that these were only one difference in the material structure of the PANI/PAA composite films synthesized by the two methods; the PANI/PAA composite film synthesized through the direct polymerization method (PANI/PAA-DP) had a larger particles size, two clear oxidation and reduction peaks, the response times for reduction and oxidation were 120 ms and 226 ms, the transmittance modulation of the PANI/PAA composite films reached 10% at 600 ~ 700 nm; the PANI/PAA composite film synthesized through the layer by layer method (PANI/PAA-LP) had a porous network structure, three clear oxidation and reduction peaks, stable electrochemical property, improved electrochromic performance, the response times for reduction and oxidation were 67 ms and 45 ms, the transmittance modulation of the PANI/PAA composite films reached 40% at 600 ~ 700 nm, respectively.

Abstract:3,4-Methylenedioxyphenol p-perfluorononenebenzonate was synthesized by esterification from p-perfluorononenebenzoyl chloride(PFNBC) and 3,4- methylenedioxy- phenol. The product was characterized by FT-IR、1H NMR、13F NMR. The effects of catalyst, reaction temperature, reaction time and the ratio of reactants on the esterification were investigated. The optimum reaction conditions of the esterification were determined as follows: n(PFNBC):n(sesamol):n(NEt3)=1:2.0:1, the reactants were agitate in DMF at -5℃ for 4h to give 3,4-methylenedioxyphenol p-perfluorononenebenzonate in the yield of 79.0 %.

Abstract:Nonylphenol polyoxypropylene polyoxyethylene oxide sulfonates (NPESO-3-4) was synthesized and content of raw materials in product was analyzed by high-performance liquid chromatography (HPLC). Surface tension, emulsifying ability, wettability and mimic oil recovery efficiency of NPESO-3-4 were measured and also compared with Nonylphenol polyoxyethylene oxide sulfonates’ (NPESO-0-4). The results showed that for surfactants in aqueous solution, the NPESO-3-4 caused a large increase in the effectiveness of surface tension reduction, while its efficiency was slightly worse than NPESO-0-4. The interfacial tensions between NPESO-3-4 and NPESO-0-4 aqueous solution/Shengli crude oil can reach the range of 10-1 mN?m-1. NPESO-3-4 could alter wettability of the surface from oil-wet to intermediate wet, but emulsifying ability and mimic oil recovery efficiency for NPESO-3-4 was significantly higher than NPESO-0-4, which indicated the Anionic-Nonionic surfactants with polyoxypropylene group were suitable for Enhanced Oil Recovery.

Abstract:Ethylene glycol Gemini sodium 2-ethyl-1-butanol sulfosuccinate was synthesized by the method of using carbonyl solid acid as the catalyst and without organic solvents in esterification and without any extra phase transfer catalysts in sulfonation at normal atmospheric pressure. The optimal synthetic conditions were as follows: in the single-esterification, n(ethylene glycol):n(maleic anhydride)=1.00:2.10, the amount of carbonyl solid acid was 2% of the amount of maleic anhydride, and reacted at 100℃ for 4.7h with the esterification rate of 99.21%(Mass fraction). In the di-esterification, n(2-ethyl-1-butanol):n(maleic anhydride)=1.30:1.00, and reacted at 210℃ for 1h with the esterification rate of 95.17%(Mass fraction). In the sulfonation, n(sodium hydrogen sulfite):n(maleic anhydride)=1.05:1.00, and reacted at 120℃ for 1h with the sulfonation rate of 100.65%( Mass fraction). The structure of the product was characterized by IR and 1HNMR. Its properties were measured: CMC=2.99×10-3mol/L , γCMC=27.96mN/m. Emulsifying power was 4.35min, permeability was 11.6s and the ability of hard water resistance was 13.3min.

Abstract:A bifunctional cycloaliphatic limonene based epoxy compound was prepared from natural D-limonene via hydroalkylation, esterification and epoxidation reaction. The structures of the intermediates and epoxy compound were characterized by 1H and 13C nuclear magnetic resonance (NMR)，MS and Fourier transform infrared (FTIR). The thermal properties of the epoxy compound cured with anhydride agents were investigated using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The glass transition temperature (Tg) of the epoxy compound cured with methylhexahydrophthalic anhydride，tetrahydrophthalic anhydride and nadic anhydride was 158 oC, 137 oC and 150 oC, respectively. The results indicated that the cured epoxy exhibited good thermal properties.

Abstract:The coumarin derivatives of phenols and ethyl acetoaceate were carried out using SO3H functionalized ionic liquid as the catalysts via Pechmann condensation. The optimum reaction condition: n(phenols):n(ethyl acetoaceate)=1:1, microwave irradiation reaction time 10 minute and reaction temperature 100℃. The high yield can reach 94％ in the presence of x([C3SO3Hmim]HSO4)=20% as catalyst, under solvent-free conditions. This method has the advantages of mild reaction conditions, easy operation, high yields and environmental begin. Moreover, the catalyst could be reused for at least four times.

Abstract:To investigate the chemical constituents of longan (Dimocarpus longan Lour.) seeds, a ceramides molecular species (compounds 12) were isolated from petroleum ether extract and a cerebroside molecular species (compounds 36) from the w(ethanol)=95% extract on longan seeds by silica gel column chromatography, Their structures were identified on the basis of physical and chemical properties and spectral analysis. compounds 12 and compounds 36 isolated identified as: Rel-(3S,4S,5S)-3-[(2′R)-2′-hydroxydocosylamino]-4-hydroxy-5-[(4′′Z)-tetradecane -4′′ -ene]-2,3,4,5-tetrahydrofuran(1), Rel-(3S,4S,5S)-3-[(2′R)-2′-hydroxytetracosanoyl- amino]-4-hydroxy-5-[(4′′Z)-tetradecane-4′′-ene]-2,3,4,5-tetrahydrofuran(2), 1-O-β-D- glucopyranosyl-(2S,3S,4R,8E)-2-[2′-hydroxylignoceroylamino]-8-octadecene-1,3,4- triol(3), 1-O-β-D-glucopyranosyl-(2S,3S,4R,8Z)-2-[2′-hydroxylignoceroylamino]-8- octadecene-1,3,4-triol(4), 1-O-β-D-glucopyranosyl-(2S,3S,4R,8E)-2-[2′-hydroxyldoc- osylamino]-8-octadecene-1,3,4-triol(5), 1-O-β-D-glucopyranosyl-(2S,3S,4R,8Z)-2-[2′ - hydroxydocosylamino]-8-octadecene-1,3,4-triol(6).

Abstract:Supercritical CO2 fluid extraction technology was used to extract camptothecin from Camptotheca acuminate seeds. With the preconditions of CO2 flux 20 L/h, the effect of different parameters such as extraction time, temperature, extraction pressure and entrainer on the supercritical carbon dioxide extraction of camptothecin was investigated. The optimum technological conditions were validated by orthogonal experiments design: extraction press 25MPa, temperature 50℃, extraction time 120 min, and entrainer 90% ethanol. Under the optimal conditions, extraction rates of camptothecin was 76.98%, content of camptothecin was 43.68% in crude extracts.

Abstract:Amino acid was extracted from the leaves of Discoleidion rufescens by acid hydrolyzed protein method and determined the contents of amino acid. The single factor experiment and response surface experiment were applied to determine the optimum production condition with the evaluation of the ratio of amino acid extraction. The results are as follows: concentration of Hydrochloric acid 6.1mol/L, ratio of liquid to material 21.6:1, hydrolysis time 22.3h, hydrolysis temperature 100℃ with activated charcoal decoloration and ion exchange chromatography, the extract rate of amino acid was 11.2% under these conditions; the amino acid content in the product was 79.7%; the total essential amino acid content was 24%.

Abstract:The essential oils which extracted by hydro distillation method was studied by GC-MS and evaluation methods during Chimonanthus praecox (L.) Link booming. The number and the contents of fragrant components of essential oils were changed during aroma releasing.The components of fragrant contents of essential oils were identified by searching the standard NIST05 database during the following three stages (buds, early spread, spread),and the variation of fragrant contents was studied as well. Results showed that the main fragrant components of different booming stages(buds, early spread, spread and final flowers) was approximately the same, whereas the relative percentage of linool increased significantly from the buds from early spread, arrived at the maximum of 11.72%.

Abstract:Memantine hydrochloride was synthesized from 1, 3-dimethyladamantane through nitration with HNO3 and N-hydroxyphthalimide, hydrogenation under 1MP hydrogen and 10% Pd-C, formation of salt with concentrated HCl. The overall yield reached 80.54%. Optimum condition of nitration was investigated, such as catalyst, quantity of HNO3, reaction time and reaction temperature. Memantine hydrochloride was recrystallized with isopropanol-water and the purity reached 99.87%. Structure of target compound was verified by 1H-NMR and HR-MS.

Abstract:Tulathromycin is a new-style macrolides antibiotic for animals. This study is intended to explore improved synthetic process route for trulathromycin using azithromycin-A as the raw material. First, protective azithromycin-A was prepared by reaction of azithromycin-A and Cbl-Cl, in this reacting the second hydroxide of azithromycin-A was protected in the presence of Cbl-Cl. Next, Cbz-protected ketone was prepared when the protective azithromycin-A was oxidized in the forth hydroxide by using Albright-Goldman method. Then protective alkene was prepared in the reacting of Witting-Horner when ketone group converted alkenyl. And then Cbz-protected epoxy compound was prepared with protective alkene was oxidized in the presence of hydrogen peroxide. After, deprotected epoxy compound was prepared with Cbz-protected epoxy compound deprotected by using Pd/C as the catalyst. Crude product of tulathromycin was prepared by reaction of deprotected epoxy compound and propylamine. Finally, the crude product was purified by phosphate and then tulathromycin was obtained in 42.0% yield with 98.0% purity determined by HPLC. This study proposed new improved preparing route, in the route, the reactions needn’t be at a low temperature compared with previous method. It can be effectively used in industrial production.

Abstract:Imidazo [1,2-b] pyridazine is the C-3 side chain of the fourth-generation cephalosporins: Cefozopran. This paper used maleic anhydride as the starting material, synthesized imidazo [1, 2-b] pyridazine through hydrazinolysis, halogenation, ammonolysis, cyclization and dehalogenation. Strong acids were applied as the reaction medium of the first step, the yield of maleic hydrazide can be reached up to 96%. 3, 6-dichloro-pyridazine was synthesized by a new one-pot method which increased the yield from 74.4% to 88%. 3-amino-6-chloro pyridazine was synthesized by microwave-assisted ammonolysis, which could shorten the reaction time from 17 hours to 0.5 hours. During the formation of the imidazole ring, with ethanol as the solvent, the use of low-cost chloroacetaldehyde could simplify the reaction process. In the hydrogenation of the 6-chloro-imidazo [1,2-b] pyridazine, palladium carbon was used as the catalyst, the reaction could be accomplished at atmospheric pressure. Since each single-step yield was higher than 80%, this synthetic route was considered to be practical in industry.

Abstract:Three Br鰊sted acidic ionic liquids including 1-methyl-3-(3-sulfopropyl)imidazolium hydrogen sulfate([SO3H-pmim]HSO4), 1-(3-sulfopropyl)pyridinium hydrogen sulfate([SO3H-ppy]HSO4) and N-(3-sulfopropyl)triethylammonium hydrogen sulfate([SO3H-ptea]HSO4) were synthesized. A one-pot reaction of o-aminoacetophenone and aromatic aldehydes in the presence of ionic liquid as an effective catalyst for the synthesis of 2-aryl-2,3-dihydro-4(1H)-quinolones was described. The activity and reusability of ionic liquid as catalyst for reaction of o-aminoacetophenone and aromatic aldehydes were investigated. The ionic liquids exhibited high catalytic activity and good reusability for reaction of o-aminoacetophenone and aromatic aldehydes, and the catalytic performance of [SO3H-ptea]HSO4 could be much better than that of others. The reaction of o-aminoacetophenone and aromatic aldehydes catalyzed by [SO3H-ptea]HSO4 could proceed well to desired product in 68.3%～95.1% yields under the conditions of solvent-free and reaction temperature 60 ℃. The ionic liquid was reused at least five times without significant decrease in activity after drying under vacuum.

Abstract:Potassium salt of 1-methylamino-1-thio-2-nitroethylene was synthesized from nitromethane, methyl isothiocyanate in the presence of macronano-K2CO3 and then reacted with dimethyl sulfate in water to give 1-methylamino-1-methylthio-2-nitroethylene. The overall yield was 86%. The effects of molar ratio of raw material, reaction temperature and reaction time on conversion rate of methyl isothiocyanate were investigated. The target products were characterized by means of FTIR and 1HNMR.

Abstract:Bifonazole as basic remedy was combined with clobetasol propionate and cinnamaldehyde to make a compound. By drafting the pseudoternary phase diagrams, optimal bifonazole nanoemulsion was chosen for quality evaluation. It was found that the mass fraction of optimal bifonazole nanoemulsion was as follows, w (bifonazole) = 1.6%, w (clobetasol propionate) = 0.05%, w (cinnamaldehyde) = 0.15%, w (Tween-80) = 29.5%, w (ethanol) = 9.8%, w (acetic ether) = 13.6%, and w (distilled water) = 45.3%. This oil-in-water nanoemulsion could be easily diluted by water, exhibited a spherical shape without adhesion or aggregation, and presented a Z-average diameter of 10.4 nm and a polydispersity index (PDI) of 0.196. After a 5-fold dilution, the average pH value was 6.1±0.3, and the corresponding zeta potential was (9.18±0.2) mV at 25 ℃. The preparation process of this compound bifonazole nanoemulsion is simple to operate, and the quality can be controlled, standing a chance of potential clinical applications.

Abstract:A kind of borate (Titled as SPNB) containing thiophosphoric acid functional group as lubricating oil additive was synthesized by n-butanol, phosphorus pentasulfide, diethanolamine, boric acid etc and its chemical structure was characterized using elemental analysis and infrared spectroscopy. The soluble stability and hydrolytic stability of the SPNB were studied in hydrogenated oil HVI H200, and its tribological and performances of suppression oil temperature rising in base oil with different mass fractions and loads were evaluated on a four-ball tester, then the worn steel surface was observed and examined by means of SEM/EDS. Results showed that the SPNB has a good soluble stability and good hydrolytic stability in the base oil. When 0.5%SPNB was added into the base oil, the wear scar diameter(WSD) of steel ball and friction coefiicient(μ) could be reduced by 24% and 20%, respectively, the pB and pD values could be incresed by 60% and 26%, respectively, which compared with the base oil, meanwhile it is good to supress oil temperature rising.

Abstract:In this paper, the polysiloxane anionic emulsion and the polyacrylate latex include silane coupling agent was prepared at first. And a high organo silicon content silicone-modified polyacrylic emulsion was synthesized by graft copolymerization reaction between polysiloxane anionic emulsion and polyacrylate latex. Results showed that when mass fraction of silicone was 20％，the polymer emulsion film was in the best performance. Compared with the polyacrylate latex film，its contact angle of silicone-acrylic emulsion film was changed from 77.5。 to 95。. Its water absorption in 24h was decreased from 4.9％ to 2.3％. Hydrophobic property was improved a lot. Furthermore, its Tg was decreased from 8.53℃ to -1.36℃. Compliance of polymer chain was improved. The silicone-acrylic emulsion of high organosilicon content can be used as a kind of hydrophobic functional polymeric material.

Abstract:Valnemulin intermediate, 14-O-[(2-Amino-1, 1-dimethylethyl)thiomethylcarbonyl]mutilin, was prepared by one-pot method with Pleuromutilin, 4-toluenesulfonyl chloride and dimethylcysteamine hydrochloride in diethyl ether. The optimum condition was given following: n(Pleuromutilin): n(4-toluene sulfonyl chloride): n(dimethyl cysteamine hydrochloride)= 1:1.1:1.1, tetrabutyl ammonium bromide was used as phase transfer catalyst, amount of tetrabutyl ammonium bromide was 1.6 g, and reaction time for 2.5 h, reaction temperature for 30 ℃, the yield of product was 91%. Orthogonal design of 4 factors at 3 levels was applied for main process conditions，results agreed with the single factor experimental data. The structure of target compound was characterized by 1HNMR, IR and melting point.

Abstract:We present here a tri-phase transfer catalysis synthesis of Sec-butyl disulfide using sec-butyl bromine, sulfur and sodium sulfide nonahydrate as the raw material, the self-made SiO2-g-PS load of quaternary ammonium salt as the tri-phase transfer catalyst. Via the orthogonal experiment, the optimum conditions were obtained as follows: n(Na2S):n(RBr)=1:0.8, the dosage of catalyst is 0.75%,reaction temperature 30℃, reaction time 9h. Repeated the experiment 3 times, the mean of yield is 57.65%. Compared with other tri-phase transfer catalyst, the catalyst this experiment used has the best catalyst effect. What's more, by repeated use 6 times, the catalytic activity did not significantly reduced. The product was confirmed by 1HNMR and FTIR.

Abstract:Methyl 3-hydroxypropanoate was synthesized by hydroesteri- fication of ethylene oxide with carbon monoxide in the presence of Co2(CO)8 catalyst and methanol solvent. The influences of different ligands, catalyst/ligand molar ratio，reaction temperature, CO pressure, and methanol dosage in the system on the reaction were investigated. The results revealed that imidazole was a good ligand for the reaction and the optimal reaction conditions were catalyst/ ligand molar ratio1:1.5, reaction temperature 75℃, CO pressure 6.0MPa, methanol/(ethylene oxide) volume ratio 5:1. Under the optimal conditions, the conversion of ethylene oxide was 92.24%, the yield of methyl 3-hydroxypropanoate was 84.35%.

Abstract:This paper focused on the preparation of a dispersant which takes rosin as raw material, then adds maleic anhydride and finally applies diethanolameine to modify to get the Maleopimaric acid diethanolamine dispersant that was used in coal water slurry (CWS). This dispersant has a lot amount of alcohol amide structures which can make water moisten the coal surface rapidly. Studies on dispersant’s effects on rheological behaviour of CWS with different concentration, pH and shear rates, Zeta potential for different concentration are carried out to analyze the interaction of dispersants and the surface of coal particles. Dispersants make viscosity of CWS lower because of homogeneous moistening of coal particles through dispersants’ hydrophobic groups connecting to the surface of coal and their hydrophilic groups connecting to water molecular, breaking coal particles gathering and increasing stability of CWS effectively.