Synthesis and Crystal Structure of （Z）-1- （3-Fluorobenzyl）-5-（（3-fluorobenzylimino）（2-hydroxy-4-methoxyphenyl）methyl）pyridin-2（1H）-one

The title compound （Z）-1-（3-fluorobenzyl）-5-（（3-fluorobenzylimino）（2-hydroxy-4- methoxyphenyl）methyl）pyridin-2（1H）-one （C27H22F2N2O3,Mr = 460.47） was synthesized and crystallized. The crystal belongs to the triclinic system,space group P1 with a = 9.951（6）,b = 10.059（6）,c = 12.927（7）A,α = 109.828（7）,β = 102.304（7）,γ = 104.898（7）°,Z = 2,V = 1110.2（11）A^3,Dc =1.377 Mg/m^3,μ（MoKα） = 0.102 mm^-1,F（000） = 480,the final R = 0.0449 and Rw = 0.1250 for 4595 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that both m-fluorobenzyl groups are diorientationally disordered because of the rotation of C–C single bond which was represented as F（1）,F（2） and F（1＇）,F（2＇）. The diorientational disorder was refined and gave the occupancies of 0.665（4） and 0.335（4） for F（1） and F（1＇）,0.631（3） and 0.369（3） for F（2） and F（2＇）. Hydrogen bonds existing in the cell link different components to stabilize the crystal structure. The active data proved that the title compound has good anti-HBV activity.     

Synthesis,Crystal Structure and Anti-ischemic Activity of(E)-1-(4-(Bis(4-methoxyphenyl)methyl)piperazin-1-yl)-3-(4-acetoxy-3-methoxyphenyl)prop-2-en-1-one

A new cinnamide derivative,(E)-1-(4-(bis(4-methoxyphenyl)methyl)piperazin-1-yl)-3-(4-acetoxy-3-methoxyphenyl)prop-2-en-1-one(C31H34N2O6,Mr = 530.60),has been synthesized by the condensation of 1-(bis(4-methoxyphenyl)methyl)piperazine and(E)-3-(4-acetoxy-3-methoxyphenyl)acrylic acid.The compound was characterized by 1H NMR,13 C NMR,H RMS and single-crystal X-ray diffraction.The crystal belongs to the orthorhombic system,space group P212121 with a = 24.946(5),b = 7.6380(15),c = 14.555(3) ?,V = 2773.3(10) ?3,Z = 4,Dc = 1.271 g/cm3,F(000) = 1128,μ = 0.088 mm-1,Mo Kα radiation(λ = 0.71073 ?),the final R = 0.0641 and w R = 0.1170.A total of 3009 unique reflections were collected,of which 1760 with I 2σ(I) were observed.Intramolecular C(17)–H(17B)···O(3) and C(22)–H(22A)···O(3) interactions as well as intermolecular C(27)–H(27A)···O(3) hydrogen bonds help to stabilize the crystal structure.The title compound was evaluated for the anti-ischemic activity in vitro and in vivo.The bioassay results indicated that the title compound displayed efficient activities against glutamine-induced neurotoxicity in PC12 cells and significantly prolonged the survival time of mice subjected to acute cerebral ischemia.     

5-甲基-3-对甲苯基-2-对氯苯硫基-1H茚酮的合成及晶体结构

单质碘与三苯基膦促进的对氯苯亚磺酸钠与1,3-二对甲苯基丙炔-1-醇的自由基加成-分子内氧化碳氢键环化的多步骤串联反应,以70%的产率得到化合物5-甲基-3-对甲苯基-2-对氯苯硫基-1H-茚酮。化合物经¹H NMR、¹³C NMR、 IR和HR-MS等表征,其结构经X-射线单晶衍射分析确证。晶体属于三斜晶系,空间群P-1,晶细胞参数：a=10.7305(7)?,b=13.0234(8)?,c=14.7071(9)?,α=105.289(3)°,β=101.273(3)°,γ=98.623(3)°,V=1899.7(2)?³,Z=4, Dc=1.318 mg/m³,μ=0.320 mm^-1,F(000)=784。结构偏离因子R₁=0.0705, wR₂=0.1903,共收集到8687个独立衍射点,其中I>2σ(I)的可观测点为5542个。     

FT-IR, FT-Raman and quantum chemical calculations of (E)-N-carbamimidoyl-4-((3,4-dimethoxybenzylidene) amino) benzenesulfonamide

FT-IR and FT-Raman spectra of (E)-N-carbamimidoyl-4-((3,4-dimethoxybenzylidene) amino) benzenesulfonamide were recorded and analyzed. The vibrational wavenumbers were computed using HF/6-31G*, B3PW91/6-31G* and B3LYP/6-31G* basis. The data obtained from vibrational wavenumber calculations are used to assign vibrational bands obtained experimentally. The results indicate that the B3LYP method is able to provide satisfactory results for predicting vibrational frequencies and structural parameters. The calculated first hyperpolarizability is comparable with the reported values of similar derivatives and is an attractive object for future studies of non-linear optics. The geometrical parameters of the title compound are in agreement with that of similar derivatives.     

Synthesis and Crystal Structure of 4-{[（1E）1- （2-Hydroxy-3-methoxyphenyl）methylidene]amino}- 1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one

The title Schiff base compound,C19H19N3O3,a derivative of antipyrine,has been synthesized and characterized by elemental analysis,IR,and single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group C2/c,with α = 27.935(5),b = 7.553(1),c =16.692(3) (A),β = 105.810(3)°,Z= 8,V= 3388.7(10) (A)3,Dc = 1.323 g/cm3,Mr = 337.37,λ(MoKα) =0.71073 (A),μ = 0.091 mm-1,F(000) = 1424,R = 0.0630 and wR = 0.1273.A total of 3513 unique reflections were collected,of which 2112 with I ＞ 2σ(I) were observed.The molecular structure adopts a trans configuration about the C=N double bond.The pyrazoline and C(1)～C(6) pheny1 ring are approximately coplanar (mean deviation from the combined plane is 0.069(3) (A)),with the dihedral angle of 9.7(2)°.The preliminary biological tests show that the compound has high antibacterial activities.     

Ruthenium(II)-2, 2′-bipyridine/1, 10-phenanthroline complexes incorporating (E)-2-(((5-((4-methoxyphenyl)ethynyl)pyridin-2-yl)imino)methyl)-4-((4-nitro phenyl)ethynyl)phenol as a ligand

Transition Metal Chemistry - A new series of hexa-coordinated Ru(II) complexes of the type [Ru(L)(phen)2]X (1a–d) and [Ru(L)(bipy)2]X (2a–d) (where...     

2-甲基-3-(4-对甲氧基苯基)-5-(3-甲氧基苯基)异噁唑啉及其生物活性

采用1,3-偶极环加成反应合成了2-甲基-3-对甲氧基苯基-5-间甲氧基苯基异噁唑啉,分离了顺、反异构体,采用核磁共振氢谱分析表征了顺反异构体的谱图行为,对异构体的生物活性进行了测定,新杀菌剂2-甲基-3-对甲氧基苯基-5-间甲氧基苯基异噁唑啉对病菌的有效成分为反式结构,顺式体为无效成分.     

Crystal structure of 4-(4'-diethylaminophenyl)-6-(4-methoxyphenyl)-(2-pyrrolidin-1-yl)-pyridine-3-carbonitrile.

4-(4'-Diethylaminophenyl)-6-(4-methoxyphenyl)-(2-pyrrolidin-1-yl)-pyridine-3-carbonitrile (DMPPC) was studied by X-ray diffraction methods due to its non-linear optical properties. The pyrrolidine and pyridine rings adopt half-chair and planar conformations, respectively. The molecules in the crystal are stabilized by C-H...O and C-H...N types of intermolecular interactions in addition to van der Waals forces.     

Synthesis and Crystal Structure of (E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl Propionate

(E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl propionate (C22H27O6N, Mr = 401.45) has been synthesized by a condensation reaction of paeonol with tyrosin methyl ester hydrochloride, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 11.91291(15), b = 9.49947(12), c = 19.8727(3) , β = 106.1104(15)°, V = 2160.60(5)3, Z = 4, Dc = 1.234 g/cm3, μ = 0.739 mm-1, F(000) = 856, R = 0.0466 and wR = 0.1461 for 3859 observed reflections with (Ⅰ> 2σ(Ⅰ)). In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking enantiomers, and such units are linked by intermolecular O(5)-H(5)…O(1) and intramolecular N(1)-H(1)…O(1) hydrogen bonds.     

Cooperative C-H…O H-bonds in ''Bay Area'' and Crystal Structure of 1-(4-Methylphenyl)- 3-(4-methoxyphenyl)-2-propene-1-one

The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) (A),β = 114.581(3)°, V= 1336.7(3) (A)3, Z = 4, Dc = 1.254 g/cm3, μ(MoKa) = 0.081 cm-1 and F(000) = 536.00. The final R and wR are 0.0527 and 0.1285, respectively for 3058 observed reflections (I ＞ 2σ(I)). In the title molecule, two phenyl rings are rotated oppositely with respect to the central part C(1)-C(2)=C(3)- C(4) (plane 3) and the dihedral angle between them is 14.8°. The phenone O(1) atom deviates from plane 3 by 0.291(A). In the crystal the molecules form H-bond chains of R21(6) and R21 (5) types similar crystals are also presented.     

Synthesis,Crystal Structure and Biological Activity of 8-（（4-（（2,3-diaminopyridin-4-yl）oxy）-3-fluorophenyl）-amino）-2-（4-fluorophenyl）-3-methyl-2,7-naphthyridin-1（2H）-one

The new title compound 8-((4-((2,3-diaminopyridin-4-yl)-oxy)-3-fluorophenyl)-amino)-2-(4-fluorophenyl)-3-methyl-2,7-naphthyridin-1(2H)-one(C26H20F2N6O2, Mr = 486.48) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 15.365(3), b = 13.144(2), c = 11.863(2), β= 108.882(3)°, Z = 4, V = 2267.0(7)3, Dc = 1.425 g/cm3, F(000) = 1008, μ = 0.105 mm-1, MoKa radiation(λ = 0.71073), R = 0.0480 and wR = 0.1294 for 3197 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the region C(substituents of 8-amino group and 3-methyl group on the 2,7-naphthyridin-1(2H)-one ring) of compound 6 are effectively planar. Intramolecular and intermolecular hydrogen bonds together with π···π interations are found in the structure. In addition, compound 6 shows potent c-Met and c-Kit kinase inhibition activities.     

Enantiomeric separation of novel anticancer agent 5-hydroxy-3-(4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-cyclopent-2-en-1-one

The enantiomers of 5-hydroxy-3-(4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-cyclopent-2-en-1-one, a novel anticancer agent, were separated by derivatisation with caronaldehyde, separation of the resulting diastereoisomers of the corresponding esters by silica gel column chromatography and regeneration of alcohols (S)-5-hydroxy-3-(4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-cyclopent-2-en-1-one and (R)-5-hydroxy-3-(4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-cyclopent-2-en-1-one under aqueous conditions. The absolute configuration of the enantiomers was determined by 1H NMR studies of the corresponding Mosher esters. Alternatively, the enantiomers were separated by preparative HPLC to collect the (S)- and (R)-5-hydroxy-3-(4-methoxyphenyl)-2-(3,4,5-trimethoxyphenyl)-cyclopent-2-en-1-ones with high purity which was comparable with that obtained by the chemical method. The details of these methods have been presented herein.     

Crystal structure, spectroscopy, and quantum chemical studies of (E)-2-[(2-chlorophenyl)iminomethyl]-4-trifluoromethoxyphenol

The Schiff base compound (E)-2-[(2-chlorophenyl)iminomethyl]-4-trifluoromethoxyphenol has been synthesized and characterized by IR, UV-vis, and X-ray single-crystal determination. The molecular geometry from X-ray experiment in the ground state has been compared using the density functional theory (DFT) with the 6-311++G(d,p) basis set. The calculated results show that the DFT can well reproduce the structure of the title compound. Using the TD-DFT method, electronic absorption spectra of the title compound have been predicted, and a good agreement is determined with the experimental ones. To investigate the tautomeric stability, optimization calculations at the B3LYP/6-311++G(d,p) level were performed for the enol and keto forms of the title compound. Calculated results reveal that its enol form is more stable than its keto form. The predicted nonlinear optical properties of the title compound are much greater than those of urea. The changes of thermodynamic properties for the formation of the title compound with the temperature ranging from 200 to 500 K have been obtained using the statistical thermodynamic method. At 298.15 K, the change of Gibbs free energy for the formation reaction of the title compound is -824.841 kJ/mol. The title compound can spontaneously be produced from the isolated monomers at room temperature. The tautomeric equilibrium constant is also computed as 3.85 × 10(-4) at 298.15 K for enol?keto tautomerization of the title compound. In addition, a molecular electrostatic potential map of the title compound was performed using the B3LYP/6-311++G(d,p) method.