Synthesis, Structural Characterization and Antimicrobial Activity of a Novel Cobalt(II) Complex Based on 3-Methyl-1-Phenyl-4-(2-Thienoyl)-Pyrazol-5-One

New cobalt(II) complex, [Co(O2C15H11N2S)2(OH2)2]∙2H2O (1∙2H2O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)2∙6H2O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H2O. Compound 1∙2H2O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H2O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H2O displayed moderate activity (10 ∙2H2O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).

Synthesis, Structural Characterization and Antimicrobial Activity of a Novel Cobalt(II) Complex Based on 3-Methyl-1-Phenyl-4-(2-Thienoyl)-Pyrazol-5-One

New cobalt(II) complex, [Co(O2C15H11N2S)2(OH2)2]∙2H2O (1∙2H2O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)2∙6H2O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H2O. Compound 1∙2H2O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H2O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H2O displayed moderate activity (10 ∙2H2O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).

The Synthesis of 7-[1-Aza-2-(dimethylamino)vinyl]-4-methylhydroquinolin-2-ones and their Isomerism in Different Solvents

The reaction of 7-amino-4-methyl-2(1H)-quinolone 1 and its 6-methyl derivative 2 with Vilsmeier reagent (DMF and POCl3) afforded 7-[1-aza-2-(dimethylamino)vinyl]-4-methyl-hydroquinolin-2-one 3 and 7-[1-aza-2-(dimethylamino)vinyl]-4,6-dimethylhydroquinolin- 2-one 4, respec-tively. H-1-NMR analysis in different solvents indicated that isomerism occurred due to hindered rotation around the (CH3)(2)N-C:N o -bond. The rotational energy barrier of 3 was calculated.

Synthesis,Bioactivity and Crystal Structure Analysis of Novel Benzo[d]isothiazol-3(2H)-ones

Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2（3H）-carboxamide （1） and N-（2-methoxyphenyl）-3-oxobenzo[d]isothiazole-2（3H）-carboxamide （2）,were synthesized from the initial compound benzo[d]isothiazol-3（2H）-one （BIT） and characterized by 1 H NMR,IR and elemental analysis,respectively.The single crystals of compounds 1 and 2 were obtained and determined by X-ray diffraction analysis.The preliminary results of biological activity experiment show that some of the title compounds exhibited a favorable antimicrobial activity.

Synthesis of some new 3-[5-(2-oxo-2H-3-chromenyl)-1,3-oxazol-2-yl]-1,3-thiazolan-4-ones as antimicrobials

A series of some new 2-imino-5-[（Z）-1-（4-methylphenyl）methylidene]-3-[5-（2-oxo-2H-3-chromenyl）-1,3-oxazol-2-yl]-1,3- thiazolan-4-ones 5a-j has been synthesized and assayed for their antibacterial activity against Gram-positive bacteria viz.Bacillus subtilis（ATCC 6633）,Staphylococcus aureus（ATCC 6538p） and Micrococcus luteus（IFC 12708）,and Gram-negative bacteria viz. Proteus vulgaris（ATCC 3851）.Salmonella typhimurium（ATCC 14028） and Escherichia coli（ATCC 25922）.Among the screened compounds,5d,5e,5f,5g,and 5j exhibited potent inhibitory activity compared to standard drug,and emerged as potential molecules for further development.

A bifunctional and recyclable catalyst:Amine and ionic liquid grafting on MOFs for the one-pot synthesis of N-aryl oxazolidin-2-ones

A bifunctional heterogeneous catalyst was designed and synthesized,denoted DMEDA/IL–NH2-MIL-101.The structure and physical-chemical characterization of DMEDA/IL–NH2-MIL-101 and its precursors were characterized by SEM,N2 adsorption-desorption,XPS,FT-IR,PXRD,elemental analysis,and TGA techniques.The date showed that the two catalytic components of N,N-dimethylethylenediamine(DMEDA)and 1-butyl-3-methylimidazolium bromide(BmimBr)were chemically immobilized in NH2-MIL-101 nanocages.The amine of DMEDA was grafted onto carrier NH2-MIL-101 by N–Cr coordinate covalent bonds and the ionic liquid of BmimBr(IL(Br-))was anchored in the NH2-MIL-101 nanocages by'ship-in-a-bottle'method,in which the amidogen of NH2-MIL-101 condensed with N,N-carbonyldiimidazole(CDI)firstly,and then alkylated with 1-bromo butane.This novel heterogeneous catalyst with two different active sites can efficiently catalyze the synthesis of N-aryl oxazolidin-2-ones from carbon dioxide(CO2),epoxides,and anilines in one-pot under mild solvent-free conditions.It not only showed good stability and recoverability after five cycles but also exhibited shape selectivity for the substrate due to the synergic catalysis of amine,ionic liquid,and NH2-MIL-101.This novel bifunctional material is a promising solid catalyst for the green synthesis of N-aryl oxazolidin-2-ones.

Synthesis and Crystal Structure of 2-Ethoxy-3-n-butyl-benzofuro [2,3-d]pyrimidin-4(3H)-one

The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4（3H）-one （C16H18N2O3, Mr = 286.32） has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167（14）, b = 13.113（1）, c = 8.378（1） A, β = 98.992（2）^o, V = 1488.4（3） A^3, Z = 4, Dc = 1.278, F（000） = 608, μ = 0.089 mm^-1, MoKa radiation （2 = 0.71073）, R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.

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.

Extraction of palladium(Ⅱ) from hydrochloride solutions with 2-n-octyl-4-isothiazolin-3-one as novel extractant

Solvent extraction of palladium （Ⅱ） from hydrochloric acid solution with 2-n-octyl-4-isothiazolin-3-one （OIT）/cyclohexane was studied. Effects of different parameters on extraction efficiency were evaluated. 99.96 % and 98.26 % palladium （Ⅱ） could be effectively extracted with 0.018 mol·L^-1 OIT/cyclohexane of 0.1 and 4.0 mol·L^-1 HCl medium, respectively. Nonpolar solvent and low acidity could improve the extracting efficiency, and successfully strip palladium （Ⅱ） from the loaded organic phase was achieved with 0.5 mol·L^-1 （NH2）2CS solution. It was proposed that the extraction of Pd com-plexes from HCl medium proceeded through the ion-association mechanism by slope method, NMR and FF-IR spectra.

Photosynthesis and Molecular Structure of 2-Amino-3H-phenoxazin-3-one

The single crystal of the title compound (C12H8N2O2, Mr = 212.20) has been obtained by oxidation of 2-aminophenol in methanol solution with irradiation of sunlight. The crystal belongs to monoclinic space group P21/c with cell dimensions of a = 12.925(2), b = 5.077(3), c = 14.768(3)? b = 99.38(1), V = 956.2(5)?, Z = 4, Dc = 1.474 g/cm3, = 0.103 mm-1, R = 0.054, wR = 0.074 for 785 observed reflections (I > 2s(I)). The molecule consists of three coplanar rings. Much different CC distances (1.494(4)?and 1.343(6) ? observed within the quinoidal ring show the pattern of bond fixation expected for the Kekule formula.

Synthesis,Crystal Structure and Cytotoxic Activities of Oxazolidin-2-one Derivatives

Four cytotoxic oxazolidin-2-one derivatives were prepared from alkynyl alcohol and isocynate with high yields of 83～95%, and their structures were characterized by IR, H-RESI-MS and NMR analysis. Meanwhile, the crystal of （Z）-4-benzylidene-3-ethyl-1-oxa-3-azaspiro[4.4] nonan-2-one （5a） was obtained and determined by X-ray single-crystal diffraction. Crystal data： monoclinic system, space group P121/c1, a = 10.9284（2）, b = 9.47510（10）, c = 14.2510（2） ？, β = 111.917（2）o, V = 1369.01（3） ？3, Z = 4, F（000） = 552.0, Dc = 1.248 Mg/m3, μ = 0.652 mm-1, R = 0.0473 and wR = 0.1207 for 2699 independent reflections （Rint = 0.0206） and 2581 observed ones （I 〉 2σ（I））.

Synthesis and Crystal Structure of 3-（2,4-Dichlorophenyl）- 4-dydroxy-5-cyclohexanyl-△3-dihydrofuran-2-one

The title compound 3-（2,4-dichlorophenyl）-4-dydroxy-3-（2,4-dichlorophenyl）-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-（2,4-dichlorophenyl-acetyl）-1-hydroxycyclo-hexane-carboxylate 4, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.8192（3）, b = 10.5053（5）, c = 10.5811（5）A,α = 71.681（10）, β = 78.905（12）, γ = 81.036（12）°, C15H14C1203, Mr = 313.18, V= 702.44（6）A3, Z = 2, De= 1.481 g/cm^3, F（000） = 324,μ = 0.465 mm^-1, S = 1.006, the final R = 0.0331 and wR = 0.1363 for 2505 observed reflections with I 〉 2σ（I） and 183 variable parameters. The crystal analysis shows that the cyclohexene unit of the title compound has a quasi-chair conformation, and a one-dimensional chain structure is formed via the intermolecular hydrogen bond O（1）-H（101）…O（2）.

The Synthesis of 3-(2'-Hydroxybutyl) isobenzofuran-1 (3H)-one

The synthesis of 3-(2'-hydroxybutyl）isobenzofuran-1(3H)-onel from phthalicanhydride via the intermediate 3-(2'-oxoethyl) isobenzofuran-1(3H)-one 6 was described．

Synthesis, Crystal Structure and Fungicidal Activity of (Z)-3,3-Dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one O-2-Chlorobenzyl Oxime Nitrate

The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481（8）, b = 9.3351（5）, c = 13.1911（7） , β = 98.9450（10）°, Z = 4, V = 1769.67（17） 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F（000） = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections （I 2σ（I））. X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.

Mannich Base Derivatives of 1,2-Benzisothiazolin-3-one: Syntheses, Crystal Structures and Bioactivities

Twelve Mannich base derivatives of 1,2-benzisothiazolin-3-one were synthesized by the reaction of 1,2-benzisothiazol-3（2H）-one （BIT） with different amines and formaldehyde. All the compounds were characterized by elemental analysis, IR spectroscopy, MS and 1H NMR. The crystal structure for 2,2＇-methylenebis（benzo[d]isothiazol-3（2H）-one） （3） has been determined by X-ray single-crystal structure analysis. Compound 3 （C15HIoN202S2） crystallizes in the monoclinic system, space group C2/c with a = 25.052（8）, b = 4.510（1）, c = 11.948（4） A, β = 100.992（4）°, V= 1325.2（7） A3, Mr = 314.37, Dc = 1.576 Mg.m-3, p = 0.25 mm-1, F（000） = 648, Z = 4, R = 0.034 and wR = 0.087. The preliminary biological test indicated that the compounds （2b, 2c） showed growth inhibitory activity against the gram-positive and gram-negative bacteria.

RING-OPENING POLYMERIZATION OF l,4-DIOXAN-2-ONE INITIATED BY LANTHANUM TRIS(2,6-DI-TERT-BUTYL-4-METHYLPHENOLATE)

The ring-opening polymerization of 1,4-dioxan-2-one （PDO） was carried out by lanthanum tris（2,6-di-tert-butyl-4- methylphenolate） （La（OAr）3） as novel single component initiaLor. The influences of polymerization reaction temperature and the molar ratio of monomer to initiator on the monomer conversion and molecular weight of poly（1,4-dioxan-2-one） （PPDO） were explored. PPDO with high viscosity average molecular weight of 1.95×10^5 can be prepared at 40℃ when [PDO]/ [La（OAr）3] molar ratio was 800. Mechanism investigation shows that the polymerization proceeds through a ＂coordination- insertion＂ mechanism with selective rupture of acyl-oxygen be,nd of PDO.

Synthesis and Crystal Structure of 5,5-Dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexene-1-one

The title compound 5,5-dimethyl-2-（4-chlorophenyl）（3-hydroxy-5,5-dimethyl- 2-cyclohexen-1-one-2-yl）methyl-3-（4-methoxyphenylamino）-2-cyclohexen-1-one has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/c with a = 9.4193（13）, b = 26.915（4）, c= 21.188（3） A, β = 101.906（3）°, V = 5256.2（13） A3, Z = 4, C60H68C12N2O8, Mr =1016.06, Dc = 1.284 g/cm3, F（000） = 2160, λ（MoKα） = 0.71073 A, μ = 0.182 mm^-1, R = 0.0530 and wR = 0.1131 for 4128 observed reflections （1 〉 2α（Ⅰ））. X-ray analysis reveals that there are two independent molecules in the unit and the cyclohexenone rings adopt different conformations. In addition, there are four intramolecular hydrogen bonds in the title molecule.

Synthesis of some new bis-3,4-dihydropyrimidin-2(1H)-ones by using silica-supported tin chloride and titanium tetrachloride

Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as the catalysts for the synthesis of bisdihydropyrimidin -2(1H)-ones from aromatic dialdehydes,1,3-dicarbonyl compounds and urea at 90℃under solvent-free conditions.