Electrocarboxylation of Anthrone to Anthracene-9-carboxylic Acid in the Presence of CO_2

Electrocarboxylation of anthrone in the presence of CO2 to anthrance-9-carboxylic acid directly was carried out. The electroreduction behavior of anthrone was examined by cyclic voltammetry in the absence and presence of CO2. Then the influences of the supporting electrolytes, temperature, electrode material and anthrone concentration on the carboxylation yield were investigated. Under the optimized conditions, anthrancene-9-carboxylic acid was obtained in a good yield（96.1%）.

A Novel Palladium(Ⅱ)Complex Self-assembled from Anthracene-9-carboxylic Acid:Synthesis,Crystal Structure and Spectroscopic Properties

A novel palladium（II） complex [（TMEDA）Pd（anca）2].2DMSO （1, TMEDA = N,N,N＇,N＇-tetramethylethylethylenediamine, anca = anthracene-9-carboxylic acid） was synthesized and characterized by single-crystal X-ray diffraction, 1H NMR, UV-Vis and fluorescence spectroscopy. The cell belongs to orthorhombic Aba2 space group with a = 19.698（7）, b = 21.045（7） c = 9.062（3） A, Z = 4, V= 3757（2） A3, C40H46N206PdS2, Mr = 821.31, D, = 1.452 g/cm3, F（000） = 1704, the final R = 0.0272, wR = 0.0667 and GOOF = 0.999. Complex 1 exhibits an interesting distorted clip-shaped molecular configuration which is stabilized by intramolecular C-H...O hydrogen bonds. The cells are packed into a 3D supramolecular structure based on the intermolecular C-H...zr interactions which further construct the tubular channels serving as guest molecular channels to include the DMSO solvent molecules inside. Furthermore, the spectroscopic properties of 1 were also investigated.

Synthesis and Crystal Structure of a New Complex [Cu(C_(14)H_9O_3)_2(C_5H_5N)_2(C_2H_5OH)_2]

The title compound of Cu（C14H9O3）2（C5H5N）2（C2H5OH）2（1） was synthesized via the hy- drothermal reaction of CuCl2·2H2O and 9-hydroxy-fluorene-9-carboxylic acid（HHF） with pyridine, and characterized by elemental analysis and infrared spectra. The crystal belongs to triclinic, space group P1 with a = 8.8302（12）, b = 10.1625（14）, c = 12.2708（17）, α = 86.207（2）, β = 69.562（2）, γ = 64.932（2）o, V = 930.3（2） 3, Z = 1, Mr = 764.30, Dc = 1.364 g/cm3, F（000） = 399, S = 1.059 and μ（MoKα） = 0.644 mm-1. The final R = 0.0459 and wR = 0.1274 for 3414 observed reflections with I 〉 2σ（I）. The copper atom is six-coordinated by two oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, two pyridine nitrogen atoms and two ethanol oxygen atoms, forming a distorted octahedral coordination geometry. The extensive O–H···O hydrogen bonding connects the molecules to form a one-dimensional chain structure. Between adjacent one-dimensional chains, a two-dimensional layered structure was formed by fluorene ring π-π packing interaction. Between the layers, a three-dimensional structure was formed through the π-π packing interaction of the pyridine ring. Moreover, the thermal stability and photoluminescent property of the complex has been investigated.

A Facile Synthesis of 9,10-Dimethoxybenzo[6,7]- ox-epino[3,4-<i>b</i>]quinolin-13(6<i>H</i>)-one and Its Derivatives

A concise and efficient method for the synthesis of novel 9,10-imethoxybenzo[6,7]oxepino[3,4-b]quinolin13(6H)-one and its derivatives 7a-p has been developed via the intramolecular Friedel-Crafts acylation reactions of 6,7-dimethoxy-2-(phenoxymethyl)quinoline-3-carboxylic acids 6a-p with polyphosphoric acid (PPA) as catalyst and solvent under mild conditions. The key intermediates 6a-p were prepared through the in situ formation of ethyl 6,7-dimethoxy-2-(phenoxymethyl)quinoline-3-carboxylates 5a-p followed by hydrolysis with aqueous ethanolic sodium hydroxide solution. The novel synthetic method has the advantages of good yields, easy work-up, and environmentally friendly character, which may provide a novel highly efficient process for making quinoline and related azaheterocycle libraries.

Indole Alkaloids from the Roots of Ervatamia hainanensis

Two new indole alkaloids, named ibogamine-18-carboxylic acid, 3, 4-didehydro-7, 8-dioxo-methyl ester 1, ibogamine-18-carboxylic acid, 16, 17-didehydro-9, 17-dihydro-9-hydroxy （2-oxopropyl）-methyl ester 2, were isolated from Ervatamia hainanensis. Their structures were elucidated on the basis of spectroscopic methods.

Intercalation,Cytotoxicity,and Molecular Modeling of Acenaphtho[1,2-b]pyrrole Chromophores as a New Family of Antitumor Agents

To explore new platform for DNA intercalation and potent antitumor agent, a series of 8-oxo-8H- acenaphtho[1,2-b]pyrrole-9-carboxylic acid esters chromophores has been studied. Their intercalation geometries with DNA were rex;ealed through absorption titration, SYBR Green-DNA melt curve, circular dichroism（CD）, and docking studies. It was identified that some of the compounds could intercalate into DNA along their long axis parallel to the base-pair long axis, making right-handed B form DNA transform to A-like conformation. Their binding potency varied with the different steric hindrance. Their cytotoxicity（IC50） against MCF-7 cells was found to range between 1.3 to 40.9 umol/L by MTT assay. Interestingly, the IC50 values did not show any obvious correlation to their binding constants with DNA. The chromophore with a carboxyl group exhibited the most potency of intercalating DNA and could be the promising precursor for the future intercalator for DNA, while the bromide demonstrated the highest cytotoxic activity in this series of compounds.

青蒿中1个新的生物碱类化合物

目的研究青蒿(黄花蒿Artemisia annua)干燥地上部分的化学成分。方法综合应用HP-20、硅胶、ODS、Sephadex LH-20和半制备液相等多种色谱学方法进行分离纯化,并根据化合物的理化性质和核磁共振波谱数据进行结构鉴定。结果从青蒿干燥地上部分水提取物中分离得到了5个化合物,分别鉴定为(S)-2,6,11-trimethyl-7,8-dihydro-6H-cyclohepta[b]pyridine-9-carboxylic acid(1)、arteannoide E(2)、蚱蜢酮(3)、(6S,9S)-长寿花糖苷(4)、artemanin B(5)。结论化合物1为新的生物碱,命名为青蒿生物碱;化合物3为首次从蒿属植物中分离得到。