Synthesis and Anti-HIV Activity of Trisubstituted （3＇R, 4＇R）-3＇,4＇-Di-O-（S）-camphanoyl-（＋）-c/s-khenactone （DCK） Analogs

To further explore the potential of DCK analogs as anti-HIV drug candidates, ten new tri-substituted （3＇R,4＇R）-3＇,4＇-di-O-（S）-camphanoyl-（＋）-cis-khellactone （DCK） derivatives （4-13） were designed, synthesized, and evaluated against HIV replication in MT4 cells and H9 lympho- cytes.     

Synthesis of Novel 1-Arylsulfonyl-4-（1＇-N-2＇, 3＇, 4＇, 6＇-tetra-O-acetyl-β-D-glucopyranosyl）thiosemicarbazides

The synthesis of novel 1-arylsulfonyl -4- （1＇-N -2＇, 3＇, 4＇, 6＇-tetra-O-acetyl-β-D-gluco- pyranosyl） thiosemicarbazides via condensation of 2, 3, 4, 6-tetra-O-acetyl-β-D-glucopyranosyl isothiocyanate with substituted phenylsulfonyl hydrazines was described. Their structures and physical properties were confirmed by ^1H NMR, ^13C NMR spectra, elemental analysis and MS.     

The synthesis and photoactivated cytotoxicity of novel 5-phenyl-3- （2,2＇：5＇,2″-terthien-5-yl）-4,5-dihydro-lH-pyrazolines

A series of novel 5-phenyl-3-（2,2＇：5＇,2″-terthien-5-yl）-4,5-dihydro-lH-pyrazolines were synthesized in this report. Their photoactivated cytotoxicities on the 5podoptera litura （SL） cell line were evaluated using the MTT method. It was noticed that the inhibitory activities of all the conjugates was enhanced when irradiated with UV-A light. Compounds 4, 6 and 8 were found to be most effective with inhibition rates of 88.1%, 88.0%, and 90,5%, respectively, For compound B, the inhibition rate value was only slightly enhanced under the irradiation treatment （78.3%） compared to the dark treatment （74.8%）. The relationship analysis between structure and activity showed that the middle thiophene ring played an important role on the inhibitory activities. It was shown that these compounds could be the potential candidates for new photoactivated pesticides.     

Synthesis of a Novel Diamine 4-[（4＇-Butoxyphenoxy）carbonyl]- phenyl-3＂, 5＂-diaminobenzoate and Corresponding Polyimides

A novel diamine 4-[（4＇-butoxyphenoxy）carbonyl]phenyl-3＂,5＂-diaminobenzoate （BCDA） was synthesized from 4-butoxyphenol, 4-hydroxybenzoic acid and 3,5-dinitrobenzoic acid through four main intermediates, and a series of polyimides were also synthesized. All the intermediates and the final product were characterized by FTIR and 1H-NMR. The key step in synthesis route is selective hydrolyzation of two ester groups in 4-butoxyphenyl-4＇-acetoxybenzoate, by adjusting the reaction temperature and the concentration of ammonia, shorteding the reaction time. The properties of the novel polyimides, such as the aggregation structures, glass transition temperature, solubility and the pretilt angles, were carded out.     

A Novel Diamine, 4＇-Phenyiphenyi 4-（3＂, 5＂-Diaminobenzoyioxy）- benzoate and Longer Side-chain Polyimide

This is a part of our systematic research work on polyimides with mesogenic unit side chain. In this study, a new 4＇-phenylpbenyl 4-（3＂,5＂-diaminobenzoyloxy）benzoate and polyimide were synthesized, and characterized by FTIR, ^1H-NMR, inherent viscosity, mechanical properties, and solubility measurements. The diamine composed with mesogenic unit aryl ester groups and bipbenyl group with longer L/D ratio, was synthesized by two key steps. Firstly, the hydroxy group of 4-hydroxybenzoic acid was protected by acetoxy group for avoiding self- polymerization of 4-hydroxybenzoic acid, and then selectively hydrolyzed after esterification of carboxyl. Secondly, a selective catalysis hydrogenation was adopted to prevent the aryl ester from deoxidation. Based on this diamine, a novel polyimide was prepared by polycondensation of 4＇-phenylphenyl 4-（3＂, 5＂-diaminobenzoyloxy）benzoate and 4-aminophenyl ether（ODA） with 4, 4＇-oxydiphthalic anhydride（ODPA） in N-methyl-2-pyrrolidone （NMP）. The resulting polyimide with longer side chain showed better solubility and more regular structure. Its inherent viscosity is lower than that without side chains, but its modulus and strength not only maintained, even improved.     

Hydrothermal Synthesis and Crystal Structure of a Manganese（Ⅱ） Coordination Polymer with 1,1＇-Biphenyl-2,2＇,6,6＇-tetracarboxyl Acid and 2,2＇：6,2＇-Terpyridine Ligands

The title compound {[Mn（H2BPTC）（tpy）（H2O）]·（H2O）3}, （1, H4BPTC = 1,1＇- biphenyl-2,2＇,6,6＇-tetracarboxylic acid, tby = 2,2＇：6,2＇-terpyridine） has been synthesized by the hydrothermal reaction, and its s...     

Synthesis,Structure and Photoluminescence of a Binuclear Zinc（Ⅱ） Coordination Polymer Based on 2-Carboxycinnamic Acid and Dipyrido [3,2-a： 2＇,3 ＇-c]-phenazine

A binuclear zinc（Ⅱ） complex with 2-carboxycinnamic acid （2-ccm） and dipyrido- [3,2-a：2＇,3＇-c]phenazine （DPPZ）, {[Zn2（2-ccm）2（DPPZ）2]·2H2O}n, was synthesized and characterized by elemental analysis, IR, single-crystal X-ray diffraction, thermal gravimetry and fluo- rescent emission. It crystallizes in monoclinic, space group P21/c with a = 13.409（4）, b = 25.530（7）, c = 13.952（4） A, β = 99.554（3）°, V= 4710（2） A3, Z= 4, C56H36N8O10Zn2, Mr= 1111.67, Dc = 1.568 g/cm3, μ（MoKα） = 1.093 mm^-1, F（000） = 2272, R = 0.0422 and wR = 0.0895. In the crystal, the basic unit of 1 is a binuclear Zn2 entity which is linked by 2-ccm ligand to form a 1D double chain along the a axis. The O-H...O hydrogen bonding and π-π interactions lead to a 3D supramolecular motif. In addition, thermal and luminescent properties of complex 1 have also been investigated.     

Synthesis of anionic sulphonate-crown ether surfactants

Two sulphonate-crown ether surfactants （sodium （4＇-dodecanoyldJbenzo-18-crown-6）-4＂（5＂）-sulpho- nate, ammonium （4＇-dodecanoyldibenzo-18-crown-6）-4＂（5＂）-sulphonate） were designed and synthesized via a two-step continuous method. The products were purified and characterized by IR. 1H NMR and elemental analysis. The physicochemical properties of the surfactants were studied by fluorescence, conductivity and dynamic light scattering techniques.     

Synthesis and Magnetic Properties of Polyamide Complex Containing Bithiazole Moieties

A new polyamide containing bithiazole moieties （PTA） was synthesized by the polycondensation of 2, 2＇-diamino-4, 4＇-bithiazole （DABT） and oxalyl chloride. The polymer complex was prepared from PTA and NdC13 in DMSO. They were characterized through IR and elemental analysis. The preliminary magnetic properties of the complex PTA-Nd^3＋ was investigated, it was found that the material is a ferromagnet at low temperature.     

Regioselective Acylation of 2＇- or 3＇-Hydroxyl Group in Salicin： Hemisynthesis of Acylated Salicins

Salicin-based phenolic glycosides（PGs） are important defensive substances against herbivore feeding and have good bioactivities. In this work, a novel approach for the synthesis of salicin-based PGs has been developed, by which PGs of 2＇-O-acetylsaliein（5a）, 3＇-O-acetylsalicin（gb） and 3＇-O-benzoylsalicin（Sd） were hemisynthesized. The effects of acylation reagent, solvent and temperature on the regioselective acylation of 2＇- or 3＇-hydroxyl groups of salicin mediated by dibutyltin oxide were investigated. The optimal conditions under which the best regioselectivity reached for 5a-5d were discovered, respectively. Moreover, a tentative tin-oxygen coordination mechanism was put forward to explain the different regioselectivities shown under different conditions.     

Syntheses and Biological Activities of Novel 3-Bromo-1-（3-chloropy- ridin-2-yl）-N-hydroxy-N-aryl- 1H-pyrazole-5-carboxamides

A series of novel 3-bromo-1-（3-chloropyridin-2-yl）-N-hydroxy-N-aryl-lH-pyrazole-5-carboxamides was synthesized by the reaction of pyrazole carbonyl chloride with each of substituted phenylhydroxyamines. The latter ones were prepared in good yields by reducing substituted nitrobenzene compounds with Zn/NH4CI reductant system in alcohol. Structures of the title compounds were determined by IR, 1H NMR, and HRMS. Their insecticidal and fungicidal activities were evaluated by larvicidal test against oriental armyworm and the mycelium growth rate method, respectively.     

A New Diels-Alder Type Adduct and a New Flavone from the Stem and Root Bark of Morus mongolica

A new Diels-Alder type adduct mongolicin G （1） and a new flavone 5＇-（1＂, 1＂-dimethylallyl）-5,7,2＇,4＇-tetrahydroxyflavone （2） were isolated from the stem and root bark of Morus mongolica. Their structures were determined by spectroscopic analysis and chiroptical methods.     

2,2＂-Bipyridine Adduct of Bis（O,O＇-di（2- phenylethyl）dithiophosphato）cadmium（ll）： Synthesis, Spectroscopic Characterization, Crystal Structure and Antibacterial Activity

A new 2,2＂-bipyridine adduct of bis（O,O＇-di（2-phenylethyl）dithiophosphato） cadmium（II）, [Cd{S2P（OCH2CH2Ph）2}2＂bipy] （1, bipy -- 2,2＂-bipyridine）, was synthesized and characterized by elemental analyses, IR, UV-vis, 1H NMR, fluorescence spectroscopy, thermo-gravimetric analysis, and X-ray single-crystal diffraction. The crystal of 1 crystallizes in triclinic, space group P1 with a = 10.4607（19）, b = 11.679（2）, c = 18.480（3） A, a = 98.900（2）, β = 103.321（2）, ）, = 91.779（2）, V= 2165.2（7） A3, Dc = 1.447 g/cm3, Z = 2, C42H4404N2P2S4Cd, Mr = 943.37, F（000） = 968,μ = 0.814 mm-1, the final R = 0.0536 and wR = 0.1206 for 6275 observed reflections with 1 〉 2a（/） and R = 0.0690 and wR = 0.1339 for all data. The result shows that the Cd（1） centre is five-coordinated by two N and three S atoms in a highly distorted square pyramidal configuration. The C-H＇＂S hydrogen bonding interactions and a set of weak intermolecular r-r stacking between adjacent aromatic rings stabilize the structure and make 1 assemble into a 1D zig-zag chain. In addition, the antibacterial activities of 1 against Escherichia coli, Bacillus subtilis and Staphylococcus bacteria were also screened by disc diffusion method.     

Studies on the Synthesis of a Natural Product—Piceatannol and its Analogs

Piceatannol,(E)-3,3′,4,5′-tetrahydroxy stilbene, a natural polyhydroxy stibene, possesses many biological activities, its synthesis has been reported. We designed another route of its synthesis, which can be controlled more easily. The synthetic product was characterized by elemental analysis,IR,MS and ^1H-NMR. Its analogs were synthesized by the similar method.     

Synthesis of N,N,N-4,4＂-Di-（4-methylphenyl）-2,2＇：6＇,2＂- terpyridine-N,N,N-tris（isothiocyanato） Ruthenium（Ⅱ） and Application to Colorimetric Hg^2＋ Sensor

A terpyridine derivative DPTP [di-（4-methylphenyl）-2,2＇：6＇,2＂-terpyridine] was conveniently synthesized from 2-bromopyridine via halogen-dance reaction, Kharash coupling and Stille coupling reaction. Then its corresponding ruthenium complex Ru-DPTP [N,N,N-4,4＇＇-di-（4-methy,phenyl）-2,2＇：6＇,2＂-terpyridine-N,N,N-tris（is,-thi,cyanat,）- ruthenium（H） ammonium] was obtained and fully characterized by IR, UV-Vis, ESI MS and elemental analysis. The MLCT absorption band of Ru-DPTP was blue-shifted from 570 to 500 nm upon addition of Hg^2＋. Among a series of surveyed metal ions, the complex showed a unique recognition to Hg^2＋, indicating that it can be used as a selective colorimetric sensor for Hg^2＋.     

Synthesis and Characterization of La（OH）3 Nanorods by Hydrothermal Microemulsion Method

La（OH）3 nanorods with diameters of 20-40 nm and lengths of 200-300 nm were synthesized by a hydrothermal microemulsion method. The structure and morphology of the final products were characterized by X-ray powder diffraction （XRD）, transmission electron microscopy （TEM）, and field emission scanning electron microscope （FESEM）.     

Preparation,Crystal Structure and Theoretical Calculation of N-（Pyrimidin-2-yl）-N＇-methoxycarbonyl-thiourea

The compound, N-（pyrimidin-2-yl）-N＇-methoxycarbonyl-thiourea, has been synthesized. The single crystal structure has been determined by an X-ray diffractometer. The crystal belongs to triclinic with space group P-1 and a=0.72152（4） nm, b=0.8056（4） nm, c=0.90772（5） nm, α= 105.141（4）°, β=94.588（4）°, γ= 115.415（4）°, F（000）= 220, the unit cell volume V=0.45704（4） nm^3, the molecule number in one unit cell Z=2, the absorption coefficient μ=0.333 mm^-1, the calculated density Dc= 1.542 g/cm^3. The theoretical investigation of the title compound was carried out with B3LYP/6-311G, HF/6-311G and MP2/6-311G methods, and the atomic charges and natural bond orbital analysis were also discussed.     

Synthesis and antioxidant activities of flavonoids derivatives, troxerutin and 3’, 4’, 7-triacetoxyethoxyquercetin

Syntheses of two very important derivatives of quercetin,troxerutin and 3’,4’,7-triacetoxyethoxyquercetin were described.The latter was synthesized by highly selective esterification reaction in first time.The compounds were characterized by NMR,IR and Mass spectroscopy.Additionally,the antioxidant activities of the compounds were tested by means of improved pyrogallol autoxidation method.This was the first in using this method to test the antioxidant activities of these two compounds in vitro.The optimum system of pyorgallol autoxidation spectrophotometry was investigated and established according to the reaction rules.The assay indicated that these compounds showed noticeable antioxidant activities,and compound 2 was much more effective as a free radical scavenger than the compound 1 vitamin C was used as a reference material.     

Synthesis and antitumor activities of structure-related small molecular compounds of gambogic acid

Through simplifying the complicated skeleton of the natural product gambogic acid, two series derivatives of chromone and xanthone were synthesized and examined for their antitumor activities against several cancer cells in vitro by MTT method. The results showed that appropriate introduction of prenyl group to the small molecular compounds could elevate their antitumor activities. The structure-activities relationship of synthesized compounds certified that the bridgecore in gambogic acid was very important for keeping its antitumor activities.     

Electrospray Ionization Mass Spectra of Amino Acid Methyl Ester 5 ＇-Phosphoramidates of 2＇, 3＇-Isopropylideneuridine

Amino acid methyl ester phosphates were synthesized and determined by using positive-ion mode dectrospmy ionization mass spectrometry（ESIMS） in combination with multistage tandem mass spectrometry. The fragmentation pathways were investigated, and it was observed that most fragment ions contained the phosphoryl group. It was interesting to observe that the fragmentation pathways of the protonated molecule show some differences when compared with those of the sodium ion adduct. The methoxy group of amino acid methyl ester can migrate from the carbonyl group to the phosphoryl group in the sodium ion adduct.