A green heterogeneous catalyst for Heck reaction-chitosan-immobilized palladium complex was prepared. The catalyst exhibits high activity and stereoselectivity under the moderate reaction conditions. The catalyst can ...A green heterogeneous catalyst for Heck reaction-chitosan-immobilized palladium complex was prepared. The catalyst exhibits high activity and stereoselectivity under the moderate reaction conditions. The catalyst can be separated easily from the reaction mixture and reused after washing. Under the suitable reaction conditions, the cross-coupling of iodobenzene (ArI) with acrylic acid (AA) or acrylate can be achieved 93.3% or 99% yield of trans-cinnamic acid or trans-cinnamic ester.展开更多
The title complex bis{1-[[（3-methyl-pyridin-2-yl） amino] methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol} palladium（C_（42）H_（56）O_2N_4Pd） has been synthesized by the reaction of 1-[[（3-methyl-pyridin-2-yl）a...The title complex bis{1-[[（3-methyl-pyridin-2-yl） amino] methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol} palladium（C_（42）H_（56）O_2N_4Pd） has been synthesized by the reaction of 1-[[（3-methyl-pyridin-2-yl）amino]methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol with Pd（OAc）_2, and was characterized by IR and elemental analyses（C, H, N）. Single-crystal X-ray diffraction analysis of the complex revealed an almost parallelogram geometry of the metal center, space group P1 with a = 12.3870（13）, b = 12.9673（12）, c = 14.3998（4） ？, α = 67.53（2）, β = 75.34（2）, γ = 86.89（3）°, V = 2065.5（3） A3, M_r = 773.32, Z = 2, D_c = 1.243 g/cm^3, μ = 0.489 mm^（-1）, F（000） = 816, the final R = 0.0649 and wR = 0.1567. The compound was investigated for the catalytic behavior towards norbornene（NB） vinyl addition polymerization. And the complex exhibits high catalytic activities up to 1.668 × 10~7 g of PNB（mol of Pd）^（-1） h^（-1） with high monomer conversion using methylaluminoxane（MAO） as the cocatalyst.展开更多
The title complex, C20H17N4Pd2Cl3·0.5CH3OH, crystallizes in the triclinic system, space group Pī with α = 9.927（6）, b = 11.079（6）, c = 11.233（6） ？, a = 73.970（12）, β = 85.738（16）, γ = 83.300（12）o...The title complex, C20H17N4Pd2Cl3·0.5CH3OH, crystallizes in the triclinic system, space group Pī with α = 9.927（6）, b = 11.079（6）, c = 11.233（6） ？, a = 73.970（12）, β = 85.738（16）, γ = 83.300（12）o, V = 1178.1（11） ？3, Mr = 648.55, Z = 2, Dc = 1.520 g/cm3, μ = 1.884 mm-1, F（000） = 634, the final R = 0.0460 and wR = 0.1280. This title compound was investigated for the catalytic behavior towards norbornene （NB） vinyl addition polymerization. And the complex exhibits good catalytic activity to catalyze norbornene polymerization using MAO as a cocatalyst.展开更多
The title complex 1,3-diphenyl-2-（（quinolin-8-ylamino）methylene）propane-l,3- dione-palladium was synthesized by the reaction of 1,3-diphenyl-2-（（quinolin-8-ylamino）-methylene）propane-1,3-dione with PdCl2, and ...The title complex 1,3-diphenyl-2-（（quinolin-8-ylamino）methylene）propane-l,3- dione-palladium was synthesized by the reaction of 1,3-diphenyl-2-（（quinolin-8-ylamino）-methylene）propane-1,3-dione with PdCl2, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the orthorhombic system, space group P21212 with a = 21.838（4）, b = 8.3952（17）, c = 11.497（2） A, V= 2107.9（7） A3, C25H17C1N2O2Pd, Mr = 519.26, Z= 4, Dc= 1.636 g/cm3, H = 1.032 mm-1, F （000） = 1040, the final R = 0.0307 and wR = 0.0778. This compound was investigated for the catalytic behavior towards norbornene （NB） vinyl addition polymerization. And the complex exhibits excellent catalytic activities up to 2.18×10^8g of PNB （tool of Pd）-1 h-1 with high monomer conversion using methylaluminoxane （MAO） as the cocatalyst.展开更多
The palladium complex of the molecular complex of poly(4 vinylpyridine) with acetic acid(PVP/ HAc Pd) was prepared. Its catalytic activity for the hydrogenation of nitrobenzene was found much higher than that of the c...The palladium complex of the molecular complex of poly(4 vinylpyridine) with acetic acid(PVP/ HAc Pd) was prepared. Its catalytic activity for the hydrogenation of nitrobenzene was found much higher than that of the corresponding palladium complex of poly(4 vinylpyridine). In the presence of a strong inorganic alkali, especially potassium hydroxide, the catalytic activity is greatly improved. The suitable hydrogenation condition for PVP/HAc Pd is to use 0 1 mol/L ethanol solution of potassium hydroxide as the hydrogenation medium and the hydrogenation is carried out at 45 ℃.展开更多
Acrylonitrile reacts with aryl iodides in the presence of tri-n-butylamine and a catalytic amount of a silica-bound arsine palladium(0) complex to afford stereoselectively (E)-cinnamo- nitriles in high yields.
The title complex N,N＇-bis（2-benzoyl-3-oxobutane）-trans-l,2-diaminocyclo- hexane-palladium （C28H28N2PdO4） has been synthesized by the reaction of N,N＇-bis（2- benzoyl-3-oxobutane）-trans-l,2-diamino-cyclohexane ...The title complex N,N＇-bis（2-benzoyl-3-oxobutane）-trans-l,2-diaminocyclo- hexane-palladium （C28H28N2PdO4） has been synthesized by the reaction of N,N＇-bis（2- benzoyl-3-oxobutane）-trans-l,2-diamino-cyclohexane with PdCI2, and characterized by ele- mental analysis, IR spectrum, WAXD and TG. The spatial structures of the complex have been confirmed by single-crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic system, space group C2/c with a = 29.763（6）, b = 10.320（2）, c = 18.921（4） A, fl = 102.75（3）°, V = 5668（2） A3, C28H28N2PdO4·CH3OH, Mr = 594.97, Z = 8, Dc = 1.394 g/cm3, μ（MoKa） = 0.694 mm-1, F（000） = 2448, T= 293（2） K, R = 0.0572 and wR = 0.1347 （I〉 2σ（I））. The compound was investigated for the catalytic behavior towards norbornene （NB） vinyl addition polymerization. And the palladium complex showed excellent catalytic activity up to 9.97x 106g of PNB （mol of Pd）-1 h-1 with high monomer conversion using methylaluminoxane （MAO） as a cocatalyst.展开更多
A variety of terminal arylacetylenes have been conveniently synthesized in good to high yields via Sonogashira coupling of aryl iodides with （trimethylsilyl）acetylene catalyzed by MCM-41-supported mercapto palladium...A variety of terminal arylacetylenes have been conveniently synthesized in good to high yields via Sonogashira coupling of aryl iodides with （trimethylsilyl）acetylene catalyzed by MCM-41-supported mercapto palladium（0） complex, followed by desilylation under mild conditions. This polymeric palladium catalyst can be reused many times without any decrease in activity.展开更多
Allylic alcohols react with aryl iodides in the presence of tri-n-butylamine and a catalytic amount of a silica-bound bidentate sulfur palladium (0) complex to form 3-arylaldehydes or ketones in good yields.
Catalyst enhanced chemical vapor deposition of nickel film on high Tg polymers such as teflon(PTFE), polyimide(PI), and polysulfone(PS) was investigated by hot wall and cold wall CVD, in which Ni(dmg)_2, Ni(acac)_2, N...Catalyst enhanced chemical vapor deposition of nickel film on high Tg polymers such as teflon(PTFE), polyimide(PI), and polysulfone(PS) was investigated by hot wall and cold wall CVD, in which Ni(dmg)_2, Ni(acac)_2, Ni(hfac)_2, Ni(TMHD)_2, and Ni(cp)_2 are used as precursors, and palladium complexes are used as catalysts. The films obtained were shiny with silvery color. The Ni was metallic and the purity of Ni was about 92%-95% from XPS analysis. SEM micrographs show that the film had good morphology. The conductivity of the film was about 0.5-4 W·cm^(-1). Ni films had good adhesion with polyimide and polysulfone.展开更多
The possibility and feasibility of using supercritical fluid СО<sub>2</sub> extraction process have been investigated and described in the book as part of the task of spent catalysts regeneration. The an...The possibility and feasibility of using supercritical fluid СО<sub>2</sub> extraction process have been investigated and described in the book as part of the task of spent catalysts regeneration. The analysis of deactivating compounds has been carried out for industrial catalysts such as: 1) palladium catalyst G-58E of ethane-ethylene fraction hydrogenation;2) nickel/kieselguhr catalyst of process of separating acetylenic compounds from isoprene;3) active aluminum oxide catalyst of methyl phenyl carbinol dehydration process;4) palladium catalyst LD-265 of hydrocarbons hydrogenation process;5) nickel-molybdenum catalysts DN-3531 and Criterion 514 of kerosene hydrotreating process. The results of the study of catalyst deactivating compounds solubility in pure supercritical carbon dioxide and supercritical carbon dioxide are modified with polar additive. The results of the solubility study are described using the Peng-Robinson equation of state. The results of the implementation of the supercritical fluid СО<sub>2</sub> extraction process with respect to deactivated industrial catalyst samples have been provided. A comparison of the characteristics of samples of catalysts regenerated using the traditional approach and the SC-CO<sub>2</sub> extraction process has been conducted. The possibility of using supercritical fluid CO<sub>2</sub> impregnation process in the synthesis of a palladium catalyst has been investigated. The synthesis of palladium chloride-based organometallic complexes has been carried out. The results of the study of solubility thereof in supercritical carbon dioxide have been provided. A dynamic supercritical fluid CO<sub>2</sub> impregnation process condition has been implemented. A comparison of the characteristics of palladium catalyst samples synthesized using the conventional approach and SC-CO<sub>2</sub> impregnation process has been conducted and presented in the book.展开更多
文摘A green heterogeneous catalyst for Heck reaction-chitosan-immobilized palladium complex was prepared. The catalyst exhibits high activity and stereoselectivity under the moderate reaction conditions. The catalyst can be separated easily from the reaction mixture and reused after washing. Under the suitable reaction conditions, the cross-coupling of iodobenzene (ArI) with acrylic acid (AA) or acrylate can be achieved 93.3% or 99% yield of trans-cinnamic acid or trans-cinnamic ester.
基金Supported by the Ministry of Education of China(No.208066)the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex bis{1-[[（3-methyl-pyridin-2-yl） amino] methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol} palladium（C_（42）H_（56）O_2N_4Pd） has been synthesized by the reaction of 1-[[（3-methyl-pyridin-2-yl）amino]methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol with Pd（OAc）_2, and was characterized by IR and elemental analyses（C, H, N）. Single-crystal X-ray diffraction analysis of the complex revealed an almost parallelogram geometry of the metal center, space group P1 with a = 12.3870（13）, b = 12.9673（12）, c = 14.3998（4） ？, α = 67.53（2）, β = 75.34（2）, γ = 86.89（3）°, V = 2065.5（3） A3, M_r = 773.32, Z = 2, D_c = 1.243 g/cm^3, μ = 0.489 mm^（-1）, F（000） = 816, the final R = 0.0649 and wR = 0.1567. The compound was investigated for the catalytic behavior towards norbornene（NB） vinyl addition polymerization. And the complex exhibits high catalytic activities up to 1.668 × 10~7 g of PNB（mol of Pd）^（-1） h^（-1） with high monomer conversion using methylaluminoxane（MAO） as the cocatalyst.
基金supported by the Natural Science Foundation of Fujian Province(2010J01026)the Ministry of Education of China(No.208066)+1 种基金the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex, C20H17N4Pd2Cl3·0.5CH3OH, crystallizes in the triclinic system, space group Pī with α = 9.927（6）, b = 11.079（6）, c = 11.233（6） ？, a = 73.970（12）, β = 85.738（16）, γ = 83.300（12）o, V = 1178.1（11） ？3, Mr = 648.55, Z = 2, Dc = 1.520 g/cm3, μ = 1.884 mm-1, F（000） = 634, the final R = 0.0460 and wR = 0.1280. This title compound was investigated for the catalytic behavior towards norbornene （NB） vinyl addition polymerization. And the complex exhibits good catalytic activity to catalyze norbornene polymerization using MAO as a cocatalyst.
基金Supported by the Natural Science Foundation of Fujian Province(2010J01026)the Ministry of Education of China(No.208066)+1 种基金the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex 1,3-diphenyl-2-（（quinolin-8-ylamino）methylene）propane-l,3- dione-palladium was synthesized by the reaction of 1,3-diphenyl-2-（（quinolin-8-ylamino）-methylene）propane-1,3-dione with PdCl2, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the orthorhombic system, space group P21212 with a = 21.838（4）, b = 8.3952（17）, c = 11.497（2） A, V= 2107.9（7） A3, C25H17C1N2O2Pd, Mr = 519.26, Z= 4, Dc= 1.636 g/cm3, H = 1.032 mm-1, F （000） = 1040, the final R = 0.0307 and wR = 0.0778. This compound was investigated for the catalytic behavior towards norbornene （NB） vinyl addition polymerization. And the complex exhibits excellent catalytic activities up to 2.18×10^8g of PNB （tool of Pd）-1 h-1 with high monomer conversion using methylaluminoxane （MAO） as the cocatalyst.
基金Supported by the Outstanding Youngs Science Foudation of Henan Province(1999)
文摘The palladium complex of the molecular complex of poly(4 vinylpyridine) with acetic acid(PVP/ HAc Pd) was prepared. Its catalytic activity for the hydrogenation of nitrobenzene was found much higher than that of the corresponding palladium complex of poly(4 vinylpyridine). In the presence of a strong inorganic alkali, especially potassium hydroxide, the catalytic activity is greatly improved. The suitable hydrogenation condition for PVP/HAc Pd is to use 0 1 mol/L ethanol solution of potassium hydroxide as the hydrogenation medium and the hydrogenation is carried out at 45 ℃.
文摘Acrylonitrile reacts with aryl iodides in the presence of tri-n-butylamine and a catalytic amount of a silica-bound arsine palladium(0) complex to afford stereoselectively (E)-cinnamo- nitriles in high yields.
基金Supported by the Natural Science Foundation of Fujian Province(2010J01026)the Ministry of Education of China(No.208066)+1 种基金the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex N,N＇-bis（2-benzoyl-3-oxobutane）-trans-l,2-diaminocyclo- hexane-palladium （C28H28N2PdO4） has been synthesized by the reaction of N,N＇-bis（2- benzoyl-3-oxobutane）-trans-l,2-diamino-cyclohexane with PdCI2, and characterized by ele- mental analysis, IR spectrum, WAXD and TG. The spatial structures of the complex have been confirmed by single-crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic system, space group C2/c with a = 29.763（6）, b = 10.320（2）, c = 18.921（4） A, fl = 102.75（3）°, V = 5668（2） A3, C28H28N2PdO4·CH3OH, Mr = 594.97, Z = 8, Dc = 1.394 g/cm3, μ（MoKa） = 0.694 mm-1, F（000） = 2448, T= 293（2） K, R = 0.0572 and wR = 0.1347 （I〉 2σ（I））. The compound was investigated for the catalytic behavior towards norbornene （NB） vinyl addition polymerization. And the palladium complex showed excellent catalytic activity up to 9.97x 106g of PNB （mol of Pd）-1 h-1 with high monomer conversion using methylaluminoxane （MAO） as a cocatalyst.
基金the National Natural Science Foundation of China (No.20462002)Natural Science Foundation of Jiangxi Province (No.0420015)for financial support.
文摘A variety of terminal arylacetylenes have been conveniently synthesized in good to high yields via Sonogashira coupling of aryl iodides with （trimethylsilyl）acetylene catalyzed by MCM-41-supported mercapto palladium（0） complex, followed by desilylation under mild conditions. This polymeric palladium catalyst can be reused many times without any decrease in activity.
文摘Allylic alcohols react with aryl iodides in the presence of tri-n-butylamine and a catalytic amount of a silica-bound bidentate sulfur palladium (0) complex to form 3-arylaldehydes or ketones in good yields.
基金Funded by the National Natural Science Foundation of China(51566005)
文摘Catalyst enhanced chemical vapor deposition of nickel film on high Tg polymers such as teflon(PTFE), polyimide(PI), and polysulfone(PS) was investigated by hot wall and cold wall CVD, in which Ni(dmg)_2, Ni(acac)_2, Ni(hfac)_2, Ni(TMHD)_2, and Ni(cp)_2 are used as precursors, and palladium complexes are used as catalysts. The films obtained were shiny with silvery color. The Ni was metallic and the purity of Ni was about 92%-95% from XPS analysis. SEM micrographs show that the film had good morphology. The conductivity of the film was about 0.5-4 W·cm^(-1). Ni films had good adhesion with polyimide and polysulfone.
文摘The possibility and feasibility of using supercritical fluid СО<sub>2</sub> extraction process have been investigated and described in the book as part of the task of spent catalysts regeneration. The analysis of deactivating compounds has been carried out for industrial catalysts such as: 1) palladium catalyst G-58E of ethane-ethylene fraction hydrogenation;2) nickel/kieselguhr catalyst of process of separating acetylenic compounds from isoprene;3) active aluminum oxide catalyst of methyl phenyl carbinol dehydration process;4) palladium catalyst LD-265 of hydrocarbons hydrogenation process;5) nickel-molybdenum catalysts DN-3531 and Criterion 514 of kerosene hydrotreating process. The results of the study of catalyst deactivating compounds solubility in pure supercritical carbon dioxide and supercritical carbon dioxide are modified with polar additive. The results of the solubility study are described using the Peng-Robinson equation of state. The results of the implementation of the supercritical fluid СО<sub>2</sub> extraction process with respect to deactivated industrial catalyst samples have been provided. A comparison of the characteristics of samples of catalysts regenerated using the traditional approach and the SC-CO<sub>2</sub> extraction process has been conducted. The possibility of using supercritical fluid CO<sub>2</sub> impregnation process in the synthesis of a palladium catalyst has been investigated. The synthesis of palladium chloride-based organometallic complexes has been carried out. The results of the study of solubility thereof in supercritical carbon dioxide have been provided. A dynamic supercritical fluid CO<sub>2</sub> impregnation process condition has been implemented. A comparison of the characteristics of palladium catalyst samples synthesized using the conventional approach and SC-CO<sub>2</sub> impregnation process has been conducted and presented in the book.
