Formation of Hybrid Ring Structure of Cyanurate/Isocyanurate in the Reaction be-tween 2,4,6-Tris(4-Phenyl-Phenoxy)-1, 3,5-Triazine and Phenyl Glycidyl Ether

Reaction products of 2,4,6-tris(4-phenyl-phenoxy)-1,3,5-triazine derived from 4-phenylphenol cyanate ester and phenyl glycidyl ether were analyzed. In addition to an isocyanurate compound and an oxazolidone compound which were well known as reaction products of cyanate esters and epoxy resins, compounds with hybrid ring structure of cyanurate/isocyanurate were determined. Gibbs free energies of the compound having hybrid ring structure of cyanurate/isocyanurate with two isocyanurate moiety were found to be lower than that of the compound with cyanurate ring structure through calculations. Calculation data supported the existence of hybrid ring structure of cy-anurate/isocyanurate. It was revealed that isomerization from cyanurate to isocyanurate occurs via hybrid ring structure of cyanurate/isocyanurate in the reaction of aryl cyanurate and epoxy.

Wet 2,4,6-trichloro-1,3,5-triazine(TCT) as an efficient catalyst for the synthesis of 2,4,6-triarylpyridines under solvent-free conditions

An efficient one-pot synthesis of 2,4,6-triarylpyridines has been described.This involves the three-component reaction of aldehydes,ketones and ammonium acetate in the presence of a catalytic amount of wet 2,4,6-trichloro-1,3,5-triazine（TCT） under solvent-free condition at 130℃.

Syntheses and Characterization of Two New Alkaline Earth Metal-organic Topological Frameworks with 3-Amino-1H-1,2,4-triazole-5-carboxylate

Two new alkaline earth metal coordination polymers constructed from the deriva-tive of 1,2,4-triazole are presented herein,namely,{[Sr（AmTAZAc）2（H2O）]}（1） and {[Ba（AmTAZAc）2（H2O）]}（2）（AmTAZAc = 3-amino-1H-1,2,4-triazole-5-carboxylate）,which have been synthesized by using the layering method and structurally characterized by elemental analysis,IR,and single-crystal X-ray diffraction.Complexes 1 and 2 are isostructural,and both crystallize in the orthorhombic system,space group Fdd2.X-ray structural analysis shows that 1 or 2 has an intriguing 3-D infinite network of（318.438.510） topology based on a 2-D sheet structure of（4,4） net.The result shows that noncovalent interactions play an important role in strengthening the whole structures of the compounds.

Synthesis and Biological Activity Study of New Schiff and Mannich Base Ligands Derived from Isatin and 3-Amino-1,2,4-triazole and Their Metal Complexes

Two new Mannich and Schiff base ligands namely： （1-（3＇-amino-methyl-1＇（H）-1＇,2＇,4＇-triazole）-3-（1＇（H）-l＇,2＇,4＇- triazole-3＇-yl） iminoisatin （Lt） and l-morpholinomethyl-3-（1＇（H）-1＇,2＇,4＇-triazolyl）iminoisatin （LII） were prepared from condensation reaction of the new Schiff base 3-（l＇（H）-l＇,2＇,4＇-triazole-3＇-yl）iminoisatin （SBH） （0.01 mol） with formaldehyde and 3-amino-l,2,4-triazole （3-At） or with formaldehyde and morpholine （0.01 mole each） respectively. Structures were characterized by tH NMR, CHN analyses, mass spectra and IR spectra. Metal complexes were synthesized by heating each ligand （0.02 mo with metal salts （0.01 moo in ethanol or ethanol： acetone mixture respectively. The formula of metal complexes were suggested depending on CHN and thermal analyses, metal and chloride contents, IR and UV-visible spectra, magnetic moments （laefr） and conductivity measurements. All complexes were of octahedral geometry except palladium （II） complexes which were square planar. The two ligands and some selected metal complexes showed various antibacterial and cytotoxic effects.

Theoretical Study on the Reaction Mechanism of 2-Methoxybenzaldehyde,4-Bromo-indanone,Malononitrile and Ammonium Acetate One-pot to Form 6-(2-Methoxyphenyl)-2-amino-6-bromo-5H-indeno[1,2-b]pyridine-3-carbonitrile

The reaction mechanism of 2-methoxybenzaldehyde, 4-bromo-indanone, malononitrile and ammonium acetate one-pot to form 6-（2-methoxyphenyl）-2-amino-6-bromo-5 Hindeno[1,2-b]pyridine-3-carbonitrile was studied by density functional theory. The geometries of the reactants, transition states, intermediates and products were optimized at the PW91/DNP level. Vibration analysis was carried out to confirm the transition state structure. Reaction pathways were investigated in this study. The result indicates that the reaction Re→ TSB1→IMB1→ TSB2→ IMB2→TSB3→IMB3→TSB4→IMB4→TSB5→IMB5→TSB6→IMB6→TSB7→IMB7→ TSB8→IMB8→TSB9→IMB9→P2 is the main pathway, the activation energy of which is the lowest. The dominant product predicted theoretically is in agreement with the experiment results.

Selenium-catalyzed oxidative carbonylation of 2-aminobenzyl alcohol to give 1,4-dihydro-2H-3,1-benzoxazin-2-one

An efficient,economical,and phosgene-free approach was developed for the preparation of l,4-dihydro-2H-3,l-benzoxazin-2-one from 2-aminobenzyl alcohol.In terms of its key features,this reaction uses the cheap and recyclable non-metal selenium as a catalyst instead of the noble metal palladium;carbon monoxide as a carbonylation agent instead of virulent phosgene or one of its derivatives;and oxygen as an oxidant.The selenium-catalyzed oxidative carbonylation reaction of2-aminobenzyl alcohol proceeded efficiently in a single pot in the presence of triethylamine to afford l,4-dihydro-2H-3,l-benzoxazin-2-one in 87%yield.Furthermore,the selenium catalyst was readily recovered and recycled,affording a product yield of 80%after five cycles.

Differential protein expression in substantia nigra induced by 1-methyl-4-phenyl-1, 2, 3, 6-tetrahydropyridine in a mouse model of chronic Parkinson’s disease

BACKGROUND： To date, a complete protein expression profile of the midbrain substantia nigra in a mouse model of chronic Parkinson＇s disease, induced by 1-methyl-4-phenyl-1, 2, 3, 6-tetrahydropyridine （MPTP）, does not exist. In addition, there are no reports of analysis of differential protein expression. OBJECTIVE： To separate and evaluate MPTP-induced differential protein expression through the use of proteomics in the substantia nigra of a mouse model of chronic Parkinson＇s disease. DESIGN： Randomized controlled animal study. SETTING： Department of Neurology, the First Affiliated Hospital, Chongqing Medical University. MATERIALS： Sixteen 8-10-week old, healthy, male, C57BL mice, weighing 20-25 g, and of clean grade, were provided by the Experimental Animal Center of Chongqing Medical University. The experimental animals were disposed according to ethical criteria. MPTP was provided by Sigma Company, USA; Pdquest 2D image analysis software and gelatum/irradiance image analysis system （ChemiDoc XRS） by Bio-Rad, USA; and Voyager DE-PROMALD1-TOF-MS mass spectroscopy analyzer by AB1 Company, USA. METHODS： This study was performed in Chongqing Neurological Laboratory between November 2006 and July 2007. Mice were randomly divided into model and control groups, with 8 mice in each group. Mice in the model group were received a subcutaneous injection of MPTP （25 mg＆g）, twice a week, for five successive weeks, to establish a chronic Parkinson＇s disease model. Mice in the control group received the same volume of a subcutaneous saline injection at the same time points. Mice were sacrificed by anesthesia to rapidly obtain the midbrain for protein separation of the substantia nigra. MAIN OUTCOME MEASURES： （1） 2-ED handbook （Bio-Rad Company） was referenced for two-dimensional electrophoresis, （2） PDQUEST8,0 analytical electrophoresis pattern was adopted to evaluate differential protein expression. （3） Peptide mass finger print map and data were retrieved on http：//www.prospector.ucsf.edu to compare differential substantia nigral protein expression in the two groups. RESULTS： Two-dimensional gel electrophoresis of substantia nigra tissue indicated that there were 33 differential protein expressions between the two groups. Three new proteins were evaluated, including α -enolase, which exhibited regulated expression, tumor necrosis factor ligand superfamily member 4, and cyclin-dependent kinase inhibitor 1B. CONCLUSION： There are three proteins that exhibit differential expression in the substantia nigra- α -enolase, tumor necrosis factor ligand superfamily member 4, and cyclin-dependent kinase inhibitor 1B.

Is三七中 2-(1′,2′ ,3′,4′-四羟基丁基 )-6-(2″,3″,4″-三羟基丁基 )吡嗪的分离、纯化和结构鉴定(英文)

从三七水溶性成分中首次分离得到一个多羟基吡嗪衍生物。该化合物经MS ,NMR ,1H 1HCOSY ,13C 1HCOSY ,HMBC等鉴定其结构为 2 (1′ ,2′,3′,4′ 四羟基丁基 ) 6 (2″ ,3″ ,4″ 三羟基丁基 ) 吡嗪。将分离样品与化学合成的化合物进行了对照 。

Valence of elements in HgBa_2Ca_(n-1)Cu_nO_(2n+2+δ)(n=1, 2, 3, 4)

Valence of elements in HgBa_2Ca_(n-1)Cu_nO_(2n+2+δ)(n=1, 2, 3, 4) (both argon and oxygen annealed samples) were calculated. The result indicated for both argon and oxygen annealed samples, Hg had the lowest valence for the highest Tc sample. For fixed n, the valence of Cu in oxygen annealed samples was larger than that in argon annealed samples, indicating that oxygen annealed samples produce more carriers than argon annealed samples.

Synthesis and Crystal Structure of Methyl 2-(Diphenylamino)-4-phenyl-1,3-thiazole-5-carboxylate

The title compound, methyl 2-（diphenylamino）-4-phenyl-1,3-thiazole-5-carboxylate, was synthesized and studied by single-crystal X-ray diffraction method. The structure of the product was confirmed by IR, 1H- and 13C-NMR spectroscopy and elemental analysis. These experimental studies were supported by quantum mechanical calculations. The structure was solved in monoclinic, space group P21/c with a = 9.573（3）, b = 19.533（7）, c = 9.876（3）, β = 92.35（4）°, V = 1845.2（10）3, T = 85（2） K, Z = 4, R = 0.040 and wR = 0.089 for 6424 observed reflections with I2σ（I）.

Synthesis and Crystal Structure of Ethyl 2-(6-(1,3-Dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) Butanoate

The title compound ethyl 2-（6-（1,3-dioxo-4,5,6,7-tetrahydro-lH-isoindol-2（3H）- yl）-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4（3H）-yl） butanoate 3 was synthesized by the reaction of ethyl 2-（6-amino-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4（3H）-yl） butanoate with 4,5,6,7- tetraydrophthalic anhydride, and its structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2 1/n with a = 9.3469（2）, b = 16.7715（5）, c = 13.7153（4） A, β= 104.9680（10）°, μ = 0.107 mm^-1, Mr = 430.42, V= 2077.08（10） ,A3, Z= 4, Dc = 1.376 g/cm3, F（000） = 904, T= 296（2） K, R = 0.0508 and wR = 0.1478.

Synthesis and Structural Characterization of 2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol

2,3-Bis（hydroxymethyl）-2,3-dinitro-1,4-butanediol（C6H12N2O8） was synthesized by condensation,cyclization,oxidative dimerization and deketalization of nitromethane with a total yield of 42.4%.The structure of the title compound was characterized by 1H NMR,13C NMR,FT-IR,elementary analysis,and X-ray single-crystal diffraction analysis,which reveals that the title compound crystallizes in triclinic,space group P with a = 0.6324（2）,b = 0.6454（3）,c = 0.7062（3） nm,α= 111.550（4）,β= 95.505（4）,γ= 113.395（4）°,V = 0.23595（16） nm3,Z = 1,Mr = 240.18,Dc = 1.690 g·cm-3,μ = 0.159 mm-1,F（000） = 126,R = 0.0304 and wR = 0.0907.

The Synthesis of 2,4,6-Triisopropyl-1, 3,5-trioxane Catalyzed by Ionic Liquids

The synthesis of 2, 4, 6-triisopropyl-1, 3, 5-trioxane with high yield and desirable selec- tivity from solvent-free cyclotrimerization of isobutyraldehyde catalyzed by ionic liquids was reported in this work.

Highly efficient synthesis of 2,3-dihydroquinazolin-4(1H)-ones catalyzed by heteropoly acids in water

Heteropoly acids efficiently catalyzed the cyclocondensation reaction of anthranilamide with aldehydes in water at ambient temperature and afforded the corresponding 2,3-dihydro-4（1H）-quinazolinones compounds in good to excellent yields.This method provides mild reaction conditions and clean reaction profiles,using a small quantity of catalyst and a simple workup procedure.

Synthesis of 2-(N-formyl)-5-aryl/aryloxymethyl-1,3,4-thiadiazoles with potential bioactivity in PEG-400

An environmental benign procedure for synthesis of 2-(N-formyl)-5-aryl/aryloxymethyl-1,3,4-thiadiazoles has been developed by reaction of 2-amino-5-aryl/aryloxymethyl-1,3,4-thiadiazoles with formic acid in PEG-400.The key advantages of this protocol are the shorter reaction time,higher yields,lower cost,simple workup,and environment-friendly compared to conventional organic solvent reaction.The present method does not involve any hazardous organic solvent or catalyst.

Synthesis and Structural Characterization of a Tetranuclear Copper Complex with 2-Amino-1,3-thiazole

The title tetranuclear complex,（μ4-oxo）-hexakis（μ2-chloro）-tetrakis（2-amino-1,3-thiazole-N）-tetra-copper（ii） [Cu4（μ4-O）（μ-Cl）6L4]（1,L=2-amino-1,3-thiazole） was synthesized by the reaction of CuCl2·2H2O with 2-amino-1,3-thiazole in methanol and characterized by IR spectra and X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1 with a=9.7137（2）,b=10.7005（2）,c=14.6505（2）,α=83.9550（10）,β=82.0930（10）,γ=67.1640（10）°,V=1387.84（4）3,Mr=883.43,Z=2,μ=3.927 mm-1,Dc=2.1144 g/cm3,F（000）=868,R=0.0332 and wR=0.0814.The complex contains a tetrahedron of four CuII atoms coordinating to a central μ4-O atom,with the six edges of the tetrahedron bridged by six Cl atoms.The Cu-O bond distances range from 1.910（2） to 1.918（2）,Cu-Cl from 2.3501（11） to 2.5924（10）,and Cu-Cu from 3.1003（6） to 3.1663（6）.The coordination geometries of the four coppers distort from trigonal bipramid to tetragonal pyramid with different distortion factors.The free animo groups of the ligands result in a lot of N-H···Cl and N-H···N intra-and intermolecular hydrogen bonds.

An efficient synthesis of 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one catalyzed by recyclable solid superacid SO_4^(2-)/TiO_2 under grinding condition

An efficient synthesis of symmetrical 2,2-bis（1H-indol-3-yl）-2H-acenaphthen-1-one is achieved via a reaction of acenaphthe-nequinone and indoles catalyzed by solid superacid SO4^2-/TiO2 under solvent-free conditions at room temperature by grinding, which provides an efficient route to the synthesis of symmetrical 2,2-bis（1H-indol-3-yl）-2H-acenaphthen-1-one.This procedure offers several advantages including solvent-free conditions,excellent yields of products,simple work-up as well as reuse of catalysts which makes it a useful and attractive protocol for the synthesis of these compounds.

Ga(ClO_4)_3-catalyzed Reaction of 1,2-Diamines and α-Bromoketones:Synthesis of 2-Substituted Quinoxalines

Ga（ClO4）3-catalyzed reaction of 1,2-aryldiamines and α-bromoketones to afford 2-substituted quinoxalines in good yields is described.The reaction proceeded via grinding process with 10%（molar fraction） catalyst under solvent-free conditions at room temperature.For unsymmetrical o-phenylenediamines bearing electron-withdrawing groups,regio-selective quinoxalines were obtained.

Synthesis of M1-3xAl2O4:Eu2+x/Dy3+ 2x(M^2+= Sr^2+, Ca^2+ and Ba^2+) phosphors with long-lasting phosphorescence properties via co-precipitation method

The long afterglow fluorescent material of M1-3xAl2O4:Eu2+ x/Dy3+2x(M2+= Sr2+, Ca2+ and Ba2+) phosphors are successfully synthesized by calcining precursor obtained via co-precipitation method at 1300oC for 4 h with reducing atmosphere (20% H2 and 80% N2). The phase evolution, morphology and afterglow fluorescent properties are systematically studied by the various instruments of XRD, FE-SEM, PLE/PL spectroscopy and fluorescence decay analysis. The PL spectra shows that the Sr1-3xAl2O4:Eu2+x/Dy3+ 2x phosphors display vivid green emission at s519 nm (4f65d1!4f7 transition of Eu2+) with monitoring of the maximum excitation wavelength at s334 nm (8S7=2!6IJ transition of Eu2+), among which the optimal concentration of Eu2+ and Dy3+ is 15 at.% and 30 at.%, respectively. The color coordinates and temperature of Sr1-3xAl2O4:Eu2+ x/Dy3+ 2x phosphors are approximately at (s0.27, s0.57) and s6700 K, respectively. On the above basis, the M0:55Al2O4:Eu2+ 0:15/Dy3+ 0:3 (M2+= Ca2+ and Ba2+) phosphors is obtained by the same method. The PL spectra of these phosphors shows the strongest blue emission at s440 nm and cyan emission at s499 nm under s334 nm wavelength excitation, respectively, which are blue shifted comparing to Sr1??3xAl2O4:Eu2+ x/Dy3+ 2x phosphors. The color coordinates and temperatures of M0:55Al2O4:Eu2+ 0:15/Dy3+ 0:3 (M2+= Ca2+ and Ba2+) phosphors are approximately at (s0.18, s0.09), s2000 K and (s0.18, s0.42), s11600 K, respectively. In this work, long afterglow materials of green, blue and cyan aluminates phosphors with excellent properties have been prepared, in order to obtain wide application in the field of night automatic lighting and display.

STUDIES ON THE STRUCTURE OF 1, 2, 4-TRIAZINE-3, 5-D IONE AND ITS DERIVATIVES

Ⅰ. INTRODUCTIONSince the 1970’s, the biological interest in the photochemistry of nucleic acid base systems has led chemists to actively investigate the photoaddition reactions of pyrimidine bases to various olefins. 1, 2, 4-Triazine-3, 5-dione itself exhibits antiviral activity and can be used as antitumor agent. A series of novel compounds with azacyclobutane were formed by using photocycloaddition of C = N double bond in 1, 2, 4-triazine-3, 5-dione(6-azauracil)