Synthesis and Characterization of A Polynuclear Yttrium Trifluoroethoxide and Its Activity for Oligomerization of Phenyl Isocyanate

A polynuclear yttrium trifluoroethoxide was synthesized and its activity for the oligomerization of phenyl isocyanate was tested. Reaction of anhydrous YC13 with CF3CH2ONa in a 1 ： 3 molar ratio in THF at room temperature, after workup, gave complex 1 as colorless crystals. The composition of complex 1 is [Y（OCH2CF3）3]6ONa2（THF）12, which was identified by elemental analysis and ^1H NMR. Further X-ray structure determination reveals that complex 1 is a polynuclear ion pair compound, [Y6（μ6-O）（OCH2CF3）18]^2- [Na（THF）6]2＋ （1）. The crystal data of complex 1 are trigonal, P-3 space group, a = 1.78440（14） nm, b = 1.78440（14） nm, c = 1.27395（12） nm, γ= 120°, V=3.5129（5） nm^3, Z = 1, Dc = 1.607 mg·m^-3, μ = 2.591 mm^- 1（Mo Ka）, F（000） = 1710, R = 0.067, wR = 0. 182. Preliminary results demonstrated that complex 1 is a highly effective catalyst for the oligomerization of phenyl isocyanate.

Ruthenium(Ⅲ) chloride as an efficient catalyst for the synthesis of perimidine derivatives under mild conditions

Various biologically important perimidine derivatives have been synthesized efficiently from various ketones and naphthalene- 1,8-diamine by using a catalytic amount of RuCl_3(1 mol%).This method is a very simple and high yielding reaction for the synthesis of perimidine derivatives.

Synthesis and Characterization of the First Dinuclear Europium(Ⅱ) Complex Supported by Carbon-Bridged Biphenolate Ligand

Anhydrous EuCl3 reacted with sodium carbon-bridged biphenolate LNa2[ L = 2,2＇-methylene bis（6-tert-butyl-4- methyl-phenoxo ] in a 1 ： 1 molar ratio in THF in the presence of HMPA （HMPA = hexamethylphosphoric triamide）, then the product formed in situ was reduced by Na-K alloy to generate the divalent carbon-bridged biphenolate europium complex [ LEu （HMPA） 2 ] 2 （THF） 4 （ 1 ） in a good isolated yield. Complex 1 was fully characterized by elemental analysis, NMR and IR spectra, and X-ray structural determination. The crystal data of complex 1 are monoclinic, P2 1/c space group, a=1.6521（3） nm, b=2.8274（3） nm, c=1.2074（2） nm, β=111.723（6）°, V=5.2393（14） nm^3, Z=2, Dc= 1.259 mg·m^-3, μ = 1.304 mm^-1, F（000） = 2092, R = 0.0815, wR = 0. 1723. Complex 1 is a dimer with two Eu - O bridges. The coordination geometry of each europium atom can be best described as a distorted trigonal bipyramid.

Large scale synthesis of ZnO nanoparticles via homogeneous precipitation

In order to synthesize ZnO nanoparticles economically, industrial-grade zinc sulfate and urea were utilized to synthesize ZnO precursors in a stirred-tank reactor or a Teflon-lined autoclave at 100-180 ℃ under complete sealing condition. The ZnO precursors were calcined at 450 ℃ for 3 h to, synthesize ZnO nanoparticles. The composition of the precursors and the formation mechanism of ZnO were studied by thermogravimetric analysis and Fourier transform infrared spectroscopy. The results of X-ray diffraction, transmission electron microscopy and scanning electron microscopy of the ZnO powders demonstrate that high-purity zincite ZnO nanoparticles are synthesized. Orthogonal experiments were performed to find out the optimal conditions for the maximum yield and the minimum size. The ettect of temperature on the size ofZnO nanoparticles was investigated. The results show that a higher temperature is propitious to obtain smaller nanoparticles.

Synthesis and characterization of lanthanide complexes containing a bulky tridentate [N,N,O] Schiff base ligand

The lanthanide complexes containing a bulky tridentate [N,N,O] Schiff base ligand 3,5-But2-2-（OH）C6H2CH=N-8-C9H6N （HL） were synthesized and characterized. The reaction of anhydrous LnCl3 with NaL formed in situ in a 1：1 molar ratio in THF at room temperature afforded the lanthanide Schiff base dichloride complexes LnLCl2（DME） （Ln=Eu （1）; Sm （2））. Complexes 1 and 2 can be used as precursors for the synthesis of the lanthanide cyclopentadienyl Schiff base derivatives. The reactions of complexes 1 and 2 with one equiv of NaCH3C5H4 in THF provided the desired products LnL（CH3C5H4）CI（THF）.THF （Ln=Eu （3）; Sm （4）） in good isolated yields. These complexes were characterized by elemental analysis, IR spectra, and X-ray structural determination, in the case of complexes 3 and 4. The crystal data of complex 3 are monoclinic, P21/C space group, a=1.3370（2） nm, b=1.5190（2） nm, c=1.8910（3） nm, β=109.846（4）°, V=3.6125（8） nm^3, Z=4, Dc=1.416 mg/m^3,μ=1.847 mm^-1, F（000）=1584, R=0.0707, wR=0.1350. The crystal data of complex 4 are monoclinic, P21/c space group, a=1.3383（1） nm, b=1.5210（2） nm, c=1.8960（2） nm, β =109.878（3）°, V=3.6293（7） nm^3, Z=4, Dc=1.407 mg/m^3, μ=1.728 mm^-1, F（000）= 1580, R=0.0670, wR=0.1385.

Synthesis, Structure, and Luminescent Property of a 3-D Strontium Complex [Sr_3(pda)_2(Hpda)_2(H2O)_2]_n·2nH_2O

The title complex [Sr3（pda）2（Hpda）2（H2O）2]n·2nH2O（H2pda = pyridine-2,6-dicar- boxylic acid） has been prepared under solvothermal conditions. It has been characterized by X-ray single-crystal diffraction, IR and elemental analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 10.3795（8）, b = 9.2225（7）, c = 18.5726（14） , β = 104.377（2）o, V = 1722.2（2） 3, C28H22N4O20Sr3, Mr = 997.36, Z = 2, Dc = 1.923 g/cm3, μ = 4.722 mm-1, F（000） = 984, the final R = 0.0269 and wR = 0.0538. This complex possesses a 3-D structure which is constructed from 1-D chain motifs linked by carboxylate groups. The luminescent property of the title complex has been investigated.

Synthesis and Structural Characterization of a Ni(Ⅱ) Complex [Ni(H_2O)_4(4,4'-bipy)_2](hca)_2

The reaction of Ni（CH3COO）2.6H2O, 4-hydroxycinnamic acid （Hhca） and 4,4＇-bipyridine （bipy） ligand in water-solution afforded a mononuclear complex [Ni（H2O）4（4,4＇-bipy）2]（hca）2 which was characterized by IR, elemental analysis, TGA and single-crystal X-ray diffraction. X-ray crystallography analysis reveals that the complex is of triclinic, space group PI with a = 7.0238（14）, b = 7.2934（11）, c = 17.186（4） A, α = 87.073（13）, β = 84.354（10）, γ = 81.961（12）°, V= 866.9（3） A^3, Z = 1, Dc = 1.474 g/cm^3, F（000） = 402,μ = 62.7 mm^-1, R = 0.0411, wR = 0.0862 and GOF = 1.048. In solid state, the cation [Ni（H2O）4（4,4＇-bpy）2]^2＋ connects six nearby hca counter anions via O-H…O hydrogen bonds to form an extended 2D lattice framework and the O-…N hydrogen bonds finally link the 2D layers into an infinite 3D network.

Synthesis and Crystal Structure of 1,7,7-Trimethyl-4-(4-methoxyphenyl)-4,6,7,8-tetrahydroquinoline-2,5(1H,3H)-diones under Microwave Irradiation

The title compound （C19H23NO3） was synthesized by the one-pot reaction ofp-methoxybenzaldehyde, Meldrum＇s acid, dimedone and CH3NH3Cl （NaOAc） in ethanol under microwave irradiation without catalyst and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 8.7462（10）, b = 17.7367（19）, c = 11.5959（14） A, β = 110.981（3）°, V= 1679.6（3） A^3, Z = 4, Dc = 1.239 g/cm^3,μ（MoKa） = 0.083 mm^-1, F（000） = 672 and Mr = 313.38. The structure was refined to R = 0.0530 and wR = 0.1216. X-ray analysis reveals that the dihedral angle between plane 1 （N（1）, C（1）, C（2）, C（3）） and plane 2 （C（1）, C（2）, C（6）, C（7）, C（9）） is 3.64°, andt hat between plane 2 and plane 3 （C（11）～C（16）） is 85.33°.

Synthesis and Molecular Structure of 4-Chloromethyl-3-anilino-2-(4-methylbenzoylimido)thiazole

The title compound 2, 4-chloromethyl-3-anilino-2-（4-methyl-benzoylimido）thiazole, was prepared by the reaction of 1-p-methylbenzoyl-3-phenylaminothiourea 1 with 1,3-dichloro- acetone. The crystal is of monoclinic, space group P21/c, with a = 8.1712（15）, b = 10.998（2）, c = 19.134（4）A, β= 94.610（5）°, C18H16ClN3OS, Mr = 357.85, Z = 4, V = 1714.0（6）A^3, De= 1.387 g/cm^3, μ（MoKa） = 0.354 mm^-1, F（000） = 744, the final R = 0.0518 and wR = 0.1167 for 3189 observed reflections （I〉 2σ（I）. Its formation mechanism was proposed.

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, Characterization, and Reactivity of Amine Bis(phenolato) Cyclopentadienyl Lanthanide Complexes

（C5H5）3Ln（THF）reacted with amine bis（phenol） LH2 [ L = Me2NCH2CH2N {CH2-（2-O-C6H2-But^1-3-Me- 5）}2 ] in a 1：1 molar ratio in THF to generate the amine bis（phenolato） cyclopentadienyl lanthanide complexes LLn（C5H5） （THF）·（THF）,（Ln = La （1）, n =0; Ln = Sm（2）, n = 1） in high yields. Complexes 1 and 2 were fully characterized by elemental analysis, NMR （for 1） and IR spectra, and X-ray structural determination. The crystal data of complex 1 are monoclinic, P21/c space goup, a= 1.1595（1） nm, b = 1.8588（2） nm, c = 1.6647（1） nm, β = 98.490（2）°, V =3.5486（5） nm^3, Z =4, Dc = 1.338 mg· m^3,μ = 1240 mm^-1, F（000）= 1488, R =0.0249, wR = 0.0568. The crystal data of complex 2 are monoclinic, P21/c sp ace goup, a = 0.9692 （1） nm, b = 1.4583 （2） nm, c = 2.8192 （3） nm, = 96.805 （2）°, V = 3.9584 （7） nm^3, Z=4, Dc =1.340 mg · ma, μ = 1.524 mm^-1, F（000）= 1668, R =0.0346, wR =0.0756. The attempts failed to synthesize the amine bis（phenolate） lanthanide alkoxides by the reactions of complexes 1 and 2 with alcohols. The preliminary results revealed that complex 1 can initiate ε-caprolactone polymerization.

Synthesis and Crystal Structure of the Copper Complex {[Cu(CH_3COO)_2(bbtz)](H_2O)_2}_n

The new copper complex { [Cu（CH3COO）2（bbtz）]（H2O）2 }, 1 （bbtz = 1,4-bis（ 1,2,4- triazol-1-ylmethyl）benzene） was synthesized and the structure was determined by single-crystal X-ray diffraction. Crystal data： C16H22CuN6O6, monoclinic, space group P21/n, a = 12.589（5）, b = 6.455（2）, c = 12.677（5） A, β= 98.748（9）°, V= 1018.2（7） A^3, Mr = 457.95, Z = 2, Dc= 1.494 g/cm^3, F（000） = 474, μ = 1.118 mm^-1, R = 0.0463 and wR = 0.0939 for 1971 observed reflections with I 〉 2σ（I）. The crystal structure of 1 is a one-dimensional chain via the bridging flexible ligand bbtz.

Synthesis and Crystal Structure of a Cadmium Coordination Polymer with Dicyanamide and 1,2-Bis(1,2,4-triazol-1-yl)ethane

The new cadmium（N） coordination polymer [Cd（bte）2（dca）2]n 1 （bte = 1,2-bis（1,2,4- triazol-1-yl）ethane, dca = dicyanamide） was synthesized and characterized by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 8.7148（15）, b = 8.6142（17）, c = 15.204（3） A, fl= 92.100（10）°, V= 1140.6（4） A3, Z= 2, Mr = 572.87, Dc= 1.668 g/cm3, F（000） = 572, /t = 1.004 mm-l, the final R = 0.0654 and wR = 0.1429 for 1737 observed reflections （I 〉 2σ（I））. The cadmium atom is coordinated equatorially by four nitrogen atoms from four bte ligands and axially by two nitrogen atoms from two dca anions to adopt a distorted octahedral geometry. Each bte molecule bridges two cadmium（II） atoms. Two strands of bte molecules are wrapped around each other, and held together by cadmium（H） atoms. 1 Forms a double chain structure containing eighteen-membered Cd2（bte）2 rings.

Microwave promoted one-pot synthesis of 3-(2′-amino-3′-cyano-4′-arylpyrid-6′-yl)coumarins

A facile procedure for the synthesis of 3-（2′-amino-3′-cyano-4′-arylpyrid-6′-yl） coumarins are being reported starting from 3- acetylcoumarin, aromatic aldehydes and malononitrile. The reactions were carried out on microwave irradiation in good yield with short time and easy work-up. The structures of all the compounds have been confirmed on the basis of their analytical, IR, ^1H NMR, and mass spectral data.

Synthesis and Molecular Structure of 1,5,1',5'-Tetraphenyl-1H,1H'-3,3'-dialkylthio-bi-1,2,4-triazole

The title compound 1,5,1 ＇,5 ＇-tetraphenyl- 1H, 1H＇-3,3 ＇-dialkylthio-bi-1,2,4-triazole （2, C28H20N6S2, Mr = 504.62） was prepared by the reaction of 1-benzoyl-3-phenylaminothiourea 1 and Mn（OAc）3·2H2O in acetic acid under microwave irradiation. The crystal is of monoclinic, space group P21/c with a = 11.3931（10）, b = 16.5787（14）（c = 26.470（2） A, β = 98.274（2）°, Z = 8, V = 4947.8（8） A3, 1）, = 1.355 g/cm^3,μMoKa） = 0.245 mm^-1, F（000） = 2096, the final R = 0.0583 and wR = 0.1502 for 8705 observed reflections （I〉 20（I））. X-ray analysis reveals that the title compound is 1,5,1 ＇,5 ＇-tetraphenyl- 1 H, 1 H＇-3,3 ＇-dialkylthio-bi- 1,2,4-triazole, and its formation mechanism was proposed.

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,Crystal Structure and Luminescent Properties of [Ag(bzdmpymt)]_6·2MeOH(bzdmpymtH = 5-Benzyl-4,6-dimethylpyrimidine-2-thione)

Reaction of AgAc with bzdmpymtH in MeOH resulted in the title compound [Ag（bzdmpymt）]6-2MeOH （1.2MeOH）, which was structurally characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis. 1.2MeOH belongs to the triclinic system, space group Pi, with a = 10.930（2）, b = 11.646（2）, c = 16.794（3）A, a = 103.97（3）, β = 97.07（3）, γ = 97.94（3）°, V = 2027.2（7） A3, Z = 1, μ = 1.629 mm^-1, Dc = 1.710 mg/m3, T = 193（2） K, CsoH86Ag6N12O2S6, Mr = 2087.25, F（000） = 1044, S = 1.034, R = 0.0355 and wR = 0.0709. In 1.2MeOH, six silver（I） atoms are held together by six bzdmpymt ligands through N and S atoms to form a water-wheel-shaped structure. Each Ag atom is coordinated by two S atoms from two bzdmpymt ligands and one N atom from the third bzdmpymt ligand, giving a trigonal planar coordination geometry. Interactions between the CH3 group of bzdmpymt ligand and one pyrimidyl nitrogen atom in an adjacent molecule afford a one-dimensional hydrogen-bonding chain running along the b axis. The luminescent property of 1.2MeOH was also investigated.

Catalyst-free and solvent-free method for the synthesis of quinoxalines under microwave irradiation

A facile procedure for the synthesis, of quinoxalines is being reported starting from benzil and 1,2-diaminobenzene. The reactions were carried out catalyst-free, solvent-free and under microwave irradiation conditions in high yield （84-98%） with short time （3-6 min） and environmental benign, as well as convenient operation. The structures of all the compounds have been confirmed on the basis of their IR, 1H NMR, and/or 13C NMR, mass spectral data.

Solvent-free and catalyst-free method for the synthesis of 2,4,5-triarylimidazoles under microwave irradiation

A facile procedure for the synthesis of 2,4,5-lriarylimidazoles is being reported starting from benzil, aromatic aldehyde and ammonium acetate. The reactions were carried out with catalyst-free, solvent-free and under microwave irradiation conditions in high yield （80-99%） with short time （3-5 min） and environmental benign, as well as convenient operation. The structures of the compounds have been confirmed on the basis of their IR, 1H NMR, and/or 13C NMR, MS, and elemental analyzer.

Synthesis and Molecular Structure of Acetic Acid-3,5-diacetoxy-2-acetoxymethyl-6-(4-quinoxalin-2-yl-phenoxy)-tetrahydro-pyran-4-yl-ester

The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-（4-quinoxalin- 2-yl-phenoxy）-tetrahydro-pyran-4-yl-ester 8 （C28H28N2O10, Mr = 552.54）, has been synthesized and its crystal structure was determined by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21, a = 10.060（8）, b = 5.648（4）, c = 24.11（2）A, β = 91.078（10）°, Z = 2, V= 1369.9（19）A^3, Dc = 1.339 g/cm^3,μ（MoKa） = 1.03 cm^-1, F（000） = 580.00, T =. 193.1 Kx-9 θmax = 25.03, （△/σ）max = 0.0000, Flack = -0.0（24）, the final R = 0.0680 and wR = 0.140 （w = 1/[0.0016Fo^2 ＋ 1.00000（Fo^2）]/（4Fo^2）） for 3126 observed reflections （1 〉 20（/））. The pyranoid ring adopts chair conformation in the sugar moiety, and all of the acetyl groups are in the e bond of the pyranoid ring, so the sugar moiety is very stable.