A new hydrogen bonded Cobalt(II) Schiff base complex,?N’-(pyridine-4-carboxaldehyde) isonicotinoylhydrazone Cobalt(II), has been synthesized from isoniazid and pyridine-4-carboxaldehyde and characterized by IR spectr...A new hydrogen bonded Cobalt(II) Schiff base complex,?N’-(pyridine-4-carboxaldehyde) isonicotinoylhydrazone Cobalt(II), has been synthesized from isoniazid and pyridine-4-carboxaldehyde and characterized by IR spectroscopy, 1H-NMR, elemental analysis, TGA and single crystal X-ray structure determination. X-ray crystal structure analysis shows an octahedral complex with a metal centre coordinated to two ligand molecules through the pyridine nitrogen atoms and four water molecules and containing two nitrate groups as counter ions. The complex crystallizes in the monoclinic crystal system and P2(1)/n space group. The unit cell dimensions are: a = 7.2108(4) Å, b = 16.6020(9) Å, c = 13.0389(6) Å,α = 90°, β = 103.972(4)°, γ = 90°. The molecule is symmetrical about the cobalt centre as observed from the 1H-NMR and 13C-NMR and confirmed by the single crystal X-ray structure of the complex. Thermogravimetric analysis shows two steps decomposition of the complex to leave a metal oxide residue. The title compound is expected to be biologically active as one of the precursors (isoniazid) is a therapeutic agent with well-established clinical applications.展开更多
Two new Cu（Ⅰ） complexes [CuCl（3-PyOH）（PPh_3）_2]（1） and [Cu_2（μ-Cl）_2（4-Stpy）（Ph_3P）_3]（2）（PyOH = hydroxypyridine; stpy = styrylpyridine） with triphenylphosphine and pyridine derivatives have been s...Two new Cu（Ⅰ） complexes [CuCl（3-PyOH）（PPh_3）_2]（1） and [Cu_2（μ-Cl）_2（4-Stpy）（Ph_3P）_3]（2）（PyOH = hydroxypyridine; stpy = styrylpyridine） with triphenylphosphine and pyridine derivatives have been synthesized and characterized by elemental analysis and X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group P2_1/c with a = 9.8945（7）, b = 37.266（2）, c = 10.9461（7） A, β = 116.0750（10）°, V = 3625.3（4） A^3, Z = 4, D_c = 1.350 Mg/cm^（-3）, μ = 0.801 mm^（-1）, F（000） = 1528, the final R = 0.0320 and w R = 0.0729 for 18568 observed reflections（I 〉 2σ（I））, R（all data） = 0.0413, wR（all data） = 0.0769, completeness to theta of 25.01 is 99.9% and GOF = 1.037. Compound 2 crystallizes in monoclinic, space group P2_1/c with a = 11.290（3）, b = 20.388（5）, c = 24.092（6） A, β = 102.028（4）°, V = 5424（2） A^3, Z = 4, D_c = 1.428 Mg/cm^（-3）, μ = 1.016 mm^（-1）, F（000） = 2408, the final R = 0.0568 and w R = 0.1486 for 27644 observed reflections（I 〉 2σ（I））, R（all data） = 0.0716, wR（all data） = 0.1592, completeness to theta of 25.01 is 99.9% and GOF = 1.056. Two new Cu（I） complexes have been utilized as catalysts for N-arylation of imidazole and both showed good catalytic activity.展开更多
Imine-bridged TTF-π-pyridine derivatives, 2NTTF, 3NTTF and 4NTTF, were synthesized and the cation-binding study was performed. It is noted that with the addition of the micromolar concentration of Pb2+ to the solutio...Imine-bridged TTF-π-pyridine derivatives, 2NTTF, 3NTTF and 4NTTF, were synthesized and the cation-binding study was performed. It is noted that with the addition of the micromolar concentration of Pb2+ to the solution, these compounds display remarkable changes in solution color, 1H NMR spectra and electrochemical properties. The nitrogen atom of the imine-bridge in 2NTTF not only serves as a π-conjugated spacer but also participates in the sensing and coordinating properties.展开更多
Ethyl 4,4,4-trifluoro-3-oxo-butyrate reacted with 2,6-dimethyl-3,5-diacetyl-pyridine 1 in the presence of NaOC2H5 at 0 ℃ to give 2,6-dimethyl-3,5-bis（4,4,4-trifluoro-1,3-oxo-butyl）-pyridine （2a） in good yield. Cy...Ethyl 4,4,4-trifluoro-3-oxo-butyrate reacted with 2,6-dimethyl-3,5-diacetyl-pyridine 1 in the presence of NaOC2H5 at 0 ℃ to give 2,6-dimethyl-3,5-bis（4,4,4-trifluoro-1,3-oxo-butyl）-pyridine （2a） in good yield. Cyclization reaction of 2a and aryl imidoyl chlorides 5a--5i, obtained from chlorination of aryl oximes with N-chlorosuccimide, afforded 2,6-dimethyl-3,5-bis[（3-aryl-5-trifluoromethyl）-isoxazol-4-carbonyl]-pyridine derivatives 6a=6i.展开更多
A novel ligand, N,N＇-（2,6-pyridinedicarbonyl）bis[N-（carboxymethyl）] （Lj） was designed and synthesized starting from pyri- dine-2,6-dicarboxylic acid （I）. The ligand （L0 and ititermediate product （3） were c...A novel ligand, N,N＇-（2,6-pyridinedicarbonyl）bis[N-（carboxymethyl）] （Lj） was designed and synthesized starting from pyri- dine-2,6-dicarboxylic acid （I）. The ligand （L0 and ititermediate product （3） were characterized by 1H nuclear magnetic resonance （NMR）, Fourier transform infrared spectrometer （FT-IR） spectra and elemental analysis. Besides, four novel co-luminescence systems of Sm-La-pyridyl carboxylic acids： K4Sm（1-x）Lax（L1）C13T1H20, K12Sm2（1-x）La2x（L2）3 C16y2H2O, K6Sm20 xyLa2x（L3）C16-y3H：O and K4Sm（1-x）Lax（L4）Cl3y4H20 （x was the mole fraction of La（III） in the mixed ions, the value was 0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, respectively; Yl, Y2, Y3, Y4 were plus integer） were studied, and the mechanism of fluorescence enhancement effect was discussed detailedly.展开更多
文摘A new hydrogen bonded Cobalt(II) Schiff base complex,?N’-(pyridine-4-carboxaldehyde) isonicotinoylhydrazone Cobalt(II), has been synthesized from isoniazid and pyridine-4-carboxaldehyde and characterized by IR spectroscopy, 1H-NMR, elemental analysis, TGA and single crystal X-ray structure determination. X-ray crystal structure analysis shows an octahedral complex with a metal centre coordinated to two ligand molecules through the pyridine nitrogen atoms and four water molecules and containing two nitrate groups as counter ions. The complex crystallizes in the monoclinic crystal system and P2(1)/n space group. The unit cell dimensions are: a = 7.2108(4) Å, b = 16.6020(9) Å, c = 13.0389(6) Å,α = 90°, β = 103.972(4)°, γ = 90°. The molecule is symmetrical about the cobalt centre as observed from the 1H-NMR and 13C-NMR and confirmed by the single crystal X-ray structure of the complex. Thermogravimetric analysis shows two steps decomposition of the complex to leave a metal oxide residue. The title compound is expected to be biologically active as one of the precursors (isoniazid) is a therapeutic agent with well-established clinical applications.
基金Supported by the National Natural Science Foundation of China(NSFC 21102102)
文摘Two new Cu（Ⅰ） complexes [CuCl（3-PyOH）（PPh_3）_2]（1） and [Cu_2（μ-Cl）_2（4-Stpy）（Ph_3P）_3]（2）（PyOH = hydroxypyridine; stpy = styrylpyridine） with triphenylphosphine and pyridine derivatives have been synthesized and characterized by elemental analysis and X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group P2_1/c with a = 9.8945（7）, b = 37.266（2）, c = 10.9461（7） A, β = 116.0750（10）°, V = 3625.3（4） A^3, Z = 4, D_c = 1.350 Mg/cm^（-3）, μ = 0.801 mm^（-1）, F（000） = 1528, the final R = 0.0320 and w R = 0.0729 for 18568 observed reflections（I 〉 2σ（I））, R（all data） = 0.0413, wR（all data） = 0.0769, completeness to theta of 25.01 is 99.9% and GOF = 1.037. Compound 2 crystallizes in monoclinic, space group P2_1/c with a = 11.290（3）, b = 20.388（5）, c = 24.092（6） A, β = 102.028（4）°, V = 5424（2） A^3, Z = 4, D_c = 1.428 Mg/cm^（-3）, μ = 1.016 mm^（-1）, F（000） = 2408, the final R = 0.0568 and w R = 0.1486 for 27644 observed reflections（I 〉 2σ（I））, R（all data） = 0.0716, wR（all data） = 0.1592, completeness to theta of 25.01 is 99.9% and GOF = 1.056. Two new Cu（I） complexes have been utilized as catalysts for N-arylation of imidazole and both showed good catalytic activity.
基金Supported by the National Natural Science Foundation of China (Grant Nos. 20732007, 20728506 & 20672122)the Ministry of Science and Technology of China (Grant Nos. 2006CB806105, 2007CB808004, 2007CB936001 & 2009CB- 22008)the Bureau for Basic Research of the Chinese Academy of Sciences
文摘Imine-bridged TTF-π-pyridine derivatives, 2NTTF, 3NTTF and 4NTTF, were synthesized and the cation-binding study was performed. It is noted that with the addition of the micromolar concentration of Pb2+ to the solution, these compounds display remarkable changes in solution color, 1H NMR spectra and electrochemical properties. The nitrogen atom of the imine-bridge in 2NTTF not only serves as a π-conjugated spacer but also participates in the sensing and coordinating properties.
基金Acknowledgement The authors thank the National Natural Science Foundation of China （NNSFC） （Nos. 21072128, 21272153）, the Key Laboratory of Organofluorine Chemistry, Shanghai Institute of Organic Chemistry for financial support.
文摘Ethyl 4,4,4-trifluoro-3-oxo-butyrate reacted with 2,6-dimethyl-3,5-diacetyl-pyridine 1 in the presence of NaOC2H5 at 0 ℃ to give 2,6-dimethyl-3,5-bis（4,4,4-trifluoro-1,3-oxo-butyl）-pyridine （2a） in good yield. Cyclization reaction of 2a and aryl imidoyl chlorides 5a--5i, obtained from chlorination of aryl oximes with N-chlorosuccimide, afforded 2,6-dimethyl-3,5-bis[（3-aryl-5-trifluoromethyl）-isoxazol-4-carbonyl]-pyridine derivatives 6a=6i.
基金Project supported by the National Natural Science Foundation of China (21071152)
文摘A novel ligand, N,N＇-（2,6-pyridinedicarbonyl）bis[N-（carboxymethyl）] （Lj） was designed and synthesized starting from pyri- dine-2,6-dicarboxylic acid （I）. The ligand （L0 and ititermediate product （3） were characterized by 1H nuclear magnetic resonance （NMR）, Fourier transform infrared spectrometer （FT-IR） spectra and elemental analysis. Besides, four novel co-luminescence systems of Sm-La-pyridyl carboxylic acids： K4Sm（1-x）Lax（L1）C13T1H20, K12Sm2（1-x）La2x（L2）3 C16y2H2O, K6Sm20 xyLa2x（L3）C16-y3H：O and K4Sm（1-x）Lax（L4）Cl3y4H20 （x was the mole fraction of La（III） in the mixed ions, the value was 0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, respectively; Yl, Y2, Y3, Y4 were plus integer） were studied, and the mechanism of fluorescence enhancement effect was discussed detailedly.
