Synthesis and in vitro-Anti-hepatitis B Virus Activities of Several Ethyl 5-Hydroxy-1H-indole-3-carboxylates

A series of ethyl 5-hydroxyindole-3-earboxylates 6a-10r was designed and synthesized. The structures of all the compounds were confirmed by IR, ^1H NMR, and MS and their anti-hepatitis B virus （HBV） activities were evaluated in 2.2.15 cells. Among them, compound 7g { ethyl 5-hydroxy-2- [ （ 3-methoxyphenylsulfinyl ） methyl ] -1-methyl-4- [ （4-methylpiperazin-1-yl） methyl ]-1H-indole-3-carboxylate} displays a significant anti-HBV activity, which is more potent than the positive control lamivudine.

An efficient synthesis of 2,2′-arylmethylene bis-(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) and 1,8-dioxooctahydroxanthenes using ZnO and ZnO-acetyl chloride

2,2'-Arylmethylene bis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) 4l-s produced from reaction between dimedone with various aldehydes in acetonitrile using ZnO as a catalyst;whereas in the presence of ZnO-acetyl chloride catalysts the reaction is limited to give only 1,8-dioxo-octahydroxanthenes 3a-k in very good yields.

Synthesis of Gingerenone C and 5-Hydroxy-1-(4′-hydroxy-3-methoxyphenyl)-7-(4′′-hydroxyphenyl)-3-heptanone

The two diarylheptanoids (E)-1-(4-hydroxy-3-methoxyphenyl)-7-(4-hydroxyphenyl) hept-4-en-3-one 1 (Gingerenone C) and (±)-5-hydroxy-1-(4-hydroxy-3-methoxyphenyl)-7-(4- hydroxyphenyl)-3-heptanone 2 were synthesized from vanillin 3 and 4-hydroxybenzaldehyde 9.

Alpha-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid receptor antagonist inhibits apoptosis of retinal ganglion cells in a rabbit model of optic nerve injury

A rabbit model of traumatic optic nerve injury, established by occlusion of the optic nerve using a vascular clamp, was used to investigate the effects of alpha-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid receptor antagonist GYKI 52466 on apoptosis of retinal ganglion cells following nerve injury. Hematoxylin-eosin staining and a terminal deoxynucleotidyl transferase dUTP nick end labeling assay showed that retinal ganglion cells gradually decreased with increasing time of optic nerve injury, while GYKI 52466 could inhibit this process. The results demonstrate that following acute optic nerve injury, apoptosis of retinal ganglion cells is a programmed process, which can be inhibited by the alpha-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid receptor antagonist.

Synthesis,Crystal Structure,and Magnetic Property of One 3D Nickel Coordination Polymer Based on 2-Hydroxy-5-(3',5'-terephthalic acid)Pyridine and 1,4-Bis(1-imdazoly)benzene

One novel nickel coordination polymer, {[Ni（OTP）（bib）1.5（H2O）]·2H2O}n（1, H2 OTP = 2-hydroxy-5-（3＇,5＇-terephthalic acid） pyridine, bib = 1,4-bis（1-imdazoly）benzene）, has been synthesized and characterized by elemental analysis（EA）, IR, powder X-ray diffraction（PXRD）, and thermogravimetric（TG） analyses. The crystal of 1 crystallizes in monoclinic, space group P21/n with a = 12.2860（5）, b = 13.8246（6）, c = 19.0140（8） A, β = 104.3870（1）°, V = 3128.2（2） A3, Z = 4, C32H28N7 Ni O8, Mr = 697.32, Dc = 1.481 g/cm^3, F（000） = 1444 and μ（Mo Kα） = 0.684 mm-1. The final R = 0.0704 and w R = 0.1764 for 5485 observed reflections with I 2σ（I） and R = 0.1087 and wR = 0.2010 for all data. Topology analysis reveals that complex 1 is a 3D 2-fold interpenetrated {4^4·6^6}-nov net based on the 1D [Ni（OTP）]n chain and the 2D [Ni2（bib）3]n sql sheet. And the variable-temperature magnetic susceptibility measurements exhibit weak antiferromagnetic coupling interaction.

Synthesis, Crystal Structure and Antitumor Activity of 4-(tert-butyl)-5-(1H-1,2,4-triazol-1-yl)-N-(2-hydroxy-3,5-diiodinebenzyl)-thiazol-2-amine

The title compound, 4-（tert-butyl）-5-（1 H- 1,2,4-triazol- 1 -yl）-N-（2-hydroxy-3,5-diio- dinebenzyl）thiazol-2-amine, was synthesized via the reduction of 4-（tert-butyl）-5-（1H-l,2,4- triazol-l-yl）-N-benzylidene-thiazol-2-amine with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic system, space group P21/c with a = 7.91944（19）, b = 10.5250（3）, c = 24.4985（6） A, Z = 4, V = 2041.66（9） A3, Mr = 599.22, Dc = 1,949 Mg/m3, S = 1.120, p = 3.203 mm-1, F（000） = 1152, the final R = 0.0283 and wR = 0.0592 for 3490 observed reflections （I 〉 2σ（I））. X-ray analysis displays that the crystal water takes part in three intermolecular hydrogen bonds of O（2）-H（2A）…O（1）, O（2）-H（2B）…N（I） and N（5）-H（5）…O（2）, and an octatomic ring R^（8） is formed via intramolecular hydrogen bond of O（I）-H（IA）…N（4）. Furthermore, the I…I contacts are involved in stabilizing the overall three-dimensional network structure. The preliminary biological test shows the title compound has good antitumor activity with the IC50 value of 26 μM against the Hela cell line.

Catalytic Dehydration of 4-Hydroxy-3-hexanone to 4-Hexen-3-one over HZSM-5 Zeolite

A study on catalytic dehydration of 4-hydroxy-3-hexanone （HH） to 4-hexen-3-one （HO） was carried out through conversion of HH over HZSM-5 zeolite catalyst in a fixed-bed reactor （FBR） operating under almospheric pressure. The test indicated a relatively high activity of the HZSM-5 zeolite capable of achieving a HH conversion of 99.2% and a HO yield of 83.5%. Catalyst deactivation could be prevented by increasing the reaction temperature by 10 ＂C for every 20 h and adding 2.0% of piperidine in the feed. A catalyst stability test （for 100 h） in FBR showed that the catalyst was active even after 100 h of time-on-stream with HH conversion remaining at 99.2% and HO yield still reaching over 83.5%. Regenera- tion experiment showed that the regenerated catalyst demonstrated a catalytic performance comparable to the fresh one.

Synthesis and Crystal Structure of [2-Hydroxy-5-(4-hydroxy-3-phenyliminomethyl-benzyl)-benzylidene]-phenyl-amine

The title compound [2-hydroxy-5-（4-hydroxy-3-phenyliminomethyl-benzyl）-benzylidene]-phenyl-amine （C27H22N2O2, Mr = 406.47） was synthesized by 5,5′-methylene-bissalicylal- dehyde with aminobenezene, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 4.4026（6）, b = 1.501（13）, c = 0.95818（12） nm, β = 90.868（2）°, V= 4.2813（9） nm^3, Z= 8, Dc= 1.292 g/cm^3,μ = 0.010, F（000） = 1744, R = 0.0576 and wR = 0.1450 for 3766 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the molecule has a pair of intramolecular OH…N hydrogen bonds.

Synthesis and in vitro Anti-hepatitis B Virus Activity of Some Ethyl 5-Hydroxy-4-substituted Aminomethyl-2-sulfinylmethyl-1H-indole-3-carboxylates

A novel series of ethyl 5-hydroxy-4-substituted aminomethyl-2-sulfinylmethyl-lH-indole-3-carboxylates 8a--8j and 11e--11f was synthesized and evaluated in HepG2.2.15 cells for their anti-hepatitits B virus（HBV） activity and cytotoxicity. Among them, six compounds showed more potent inhibitory activity than lamivudine. Compound 8e exhibited the most significant anti-HBV activity with an IC50 value of 1.62 μmol/L, which was 33-times more potent than the reference drug lamivudine（IC50=54.78μmol/L）.

Determination of Trace Manganese (Ⅱ) by Its Catalytic De-colourizing Reaction On the Aerial Oxidation of 1.5-his (2-hydroxy-5-chlorophenyl)-3-cyanoformazan and Its Kinetic Reaction Mechanism

A kinetie method is described for the determination of trace amounts of mangancsc (Ⅱ)based on its catalylic effect on the aerial oxidation of 1.5-bis (2-hydroxy-5-chlorophenyl)-3-cyanofrmazan. The reaction is followed spectrophotometrically by measurin the rate of change in absorbance at 580nm. The calibration curve (rate constant vs. manganese concentration) is linearin the range of 10~200ng in 25ml solutions. Kinetic parameters of the reaction are reported. Thereare few Interferences.

Synthesis of 1,7-Bis(4-hydroxyphenyl)-3-hydroxy-1,3-heptadien-5-one

A facile synthesis of the analog of curcumin. 1,7-bis (4-hydroxyphenyl)-3-hydroxy-1.3-heptadien-5-one 1 was achieved. The key step was completed through the regioselective condensation of ketone 5 and acyl chloride 7.

Role of α-amino-3-hydroxy-5-methyl-4-isoxazole-propionic acid receptor regulation in stress-induced pain chronification

Persistent postsurgical pain is a serious issue in public health, which has received increased interest in recent years. Previous studies have reported that psychological factors promote the development of chronic postsurgical pain. However, it is unclear how chronification of postsurgical pain occurs. The α-amino-3-hydroxy-5-methyl-4-isoxazole-propionic acid receptor(AMPA) phosphorylation in the central nervous system plays a critical role in synaptic plasticity and contributes to central sensitization and chronic pain development. Here, we discuss the role of AMPA receptor regulation in stress-induced pain chronification after surgery.

CHEMISTRY OF 1,2,4—TRIAZINES XIX THE ANOMALOUS SUBSTITUTED BENZENE SULFONATION AND PROPERTIES OF NUCLEOPHILIC ATTACK ON 6-CARBON OF 3-METHYLTHIO-5-HYDROXY-1,2,4-TRIAZINE

3-Methylthio-5-hydroxy-1,2,4-triazine(1c)reacted with substituted benzenesulfonyl chloride to give 3-methylthio-5-oxy-1,2,4-triazin-6-yl pyridinium betaine(4)in anhydrous pyridine.But when NaOH/H_2O/CH_3COCH_3 or NaOH/CH_3OH were used as reactant and solvent,3-methylthio-4-substituted benzenesulfonyl-5-oxo-6-hydroxy-1,4,5,6-tetrahydro-1,2,4-triazine(6)or 1-tosyl-3-methylthio-5-oxo-6-methyloxy-1,4,5,6-tetrahydro-1,2,4-triazine(7)was obtained respectively.The above reactions show anomalous properties of nucleophilic attack on 6-carbon in 1,2,4-triazine ring.

Auxiliary Ligands Mediated One- and Two-dimensional Cd(Ⅱ) Coordination Polymers Incorporating Methyl-3- hydroxy-5-carboxy-2-Thiophenecarboxylate Ligand

Two N-donor ligands mediated Cd（Ⅱ） coordination polymers, namely,[Cd（L）（dmpz）2]n （1） and {[Cd（L）（atr）05（H20）]（H2O）}n （2） （H2L = methyl-3-hydroxy-5-carboxy-2-thiophenecarboxylate, dmpz = 3,5-dimethylpyrazole, and atr= 4-amino-l,2,4-triazole）, havebeen produced. Their structures were characterized by single-crystal X-ray diffraction analysis,elemental analyses and infrared spectra. Compound 1 possesses a one-dimensional （1D） chainstructure and is finally extended into a three-dimensional （3D） supramolecular architecturethough hydrogen bonding interactions. Compound 2 features a two-dimensional （2D） networkwith 4-connected sql topology based on dinuclear Cd（Ⅱ） clusters as nodes, which is alsoassembled into a 3D supramolecular architecture through hydrogen bonding interactions.Furthermore, compounds 1 and 2 exhibit high thermal stabilities and intense fluorescent emissionin the solid, and can be explored as potential luminescent materials.

Thermal Decomposition Behavior and Non-isothermal Decom-position Reaction of Copper(II) Salt of 4-Hydroxy-3,5-dinitro- pyridine Oxide and Its Application in Solid Rocket Propellant

The thermal decomposition behavior and kinetic parameters of the exothermic decomposition reactions of the title compound in a temperature-programmed mode have been investigated by means of DSC, TG-DTG and lower rate thermolysis/FTIR. The possible reaction mechanism was proposed. The critical temperature of thermal explo-sion was calculated. The influence of the title compound on the combustion characteristic of composite modified double base propellant containing RDX has been explored with the strand burner. The results show that the kinetic model function in differential form, apparent activation energy Ea and pre-exponential factor A of the major exo-thermic decomposition reaction are 1-a, 207.98 kJmol-1 and 1015.64 s-1, respectively. The critical temperature of thermal explosion of the compound is 312.87 ℃. The kinetic equation of the major exothermic decomposition process of the title compound at 0.1 MPa could be expressed as: ()416.422.502?d101 edTTaa-10=-. As an auxiliary catalyst, the title compound can help the main catalyst lead salt of 4-hydroxy-3,5-dinitropyridine oxide to en-hance the burning rate and reduce the pressure exponent of RDX-CMDB propellant.

Clinical features of AMPAR2 antibody-positive autoimmune encephalitis with gastrointestinal hemorrhage: a case report

Objective:To describe the clinical features of autoimmune encephalitis complicated with gastrointestinal hemorrhage.Methods:The clinical data of one patient whose initial symptom was mental abnormality were collected and the related examinations,such as cerebrospinal fluid and magnetic resonance imaging (MRI),were improved.Results: Cerebrospinal fluid examination found that anti-α-amino-3-hydroxy-5-methyl-4-isoxazole propionic acid receptor(AMPAR)2 antibody was strongly positive,although the patient had repeated gastrointestinal hemorrhage but,after hormone combined with immunoglobulin treatment,the symptoms gradual-ly improved.Conclusion:Mental disorders are not all psychosis,and autoimmune encephalitis should not be ignored.It is very important to perform anti-AMPAR encephalitis antibody test;accurate diagnosis and timely treatment can improve the prognosis.

白车轴草化学成分的分离与鉴定

目的为白车轴草(Trifolium repensL.)的药效物质基础提供依据。方法利用制备薄层、反复硅胶、Sephadex LH-20、开放ODS柱色谱等方法进行分离纯化,根据理化性质及波谱分析对分离得到的化合物进行结构鉴定。结果分离得到10个化合物,分别鉴定为伞形花内酯(umbelliferon,1)、芒柄花素(formononetin,2)、水杨酸(salicylic acid,3)、双白瑞香素(daphnoretin,4)、4′-methoxy-coumestrol(5)、trifoliol(6)、美迪紫檀素(medicarpin,7)、环阿尔廷-25-烯-3β,24ξ-二醇(cycloart-25-en-3β,24ξ-diol,8)、3β-hydroxy-7α-methoxy-24β-ethyl-cholest-5-ene(9)、soyasapogenol B(10)。结论化合物8、9为首次从车轴草属植物中分离得到,化合物1、3、4为首次从白车轴草中分离得到。

团花树皮的化学成分研究

采用硅胶、MCI和Sephadex LH-20层析方法对团花树皮的化学成分进行分离纯化,运用现代波谱技术鉴定了10个化合物:4-carboxy-3-hydroxy-5-methylphenyl 3-methoxy-4-hydroxy-5-methylbenzoate(1),谷甾醇-3-O-(6'-O-棕榈酰基)-β-D-葡萄糖苷(2),喹诺酸-3-O-α-L-鼠李糖苷(3),clethric acid(4),常春藤苷元(5),钩藤苷元C(6),morolic acid(7),咖啡酸甲酯(8),卡丹宾(9)和3α-二氢卡丹宾(10)。其中化合物1为一个新的酚性成分,化合物2～8首次从该属植物中分离得到。

A New Antioxidant Cyclic Diarylheptanoid from the Rhizomes of Zingiber officinale

The bioassay was directed to the fractionation of the methanol extract of the rhizomes of Zingiber officinale Roscoe leading to the isolation of a new antioxidant cyclic diarylheptanoid. The structure of the new compound was established as 1, 5-epoxy-3-hydroxy-1-(3,4-dihydroxy-5-methoxy-phenyl)-7-(3,4-dihydroxyphenyl) heptane (1) on the basis of MS, 1D and 2D-NMR experiments.

Studies on the Chemical Components of Clematis chinensis

Two novel compounds, clemaphenol A and dihydro-4-hydroxy-5-hyroxymethyl-2(3H)-fura-none were isolated together with eight known compounds, isoferulic acid, b-sitosterol, daucosterol, 5-hy-droxymethyl-2-furancarboxaldehyde, 5-hydroxy-4-oxo-pentanoic acid, palmitic acid, linoleic acid and anemonin from the root of Clematis chinensis Osbeck.