Triflumezopyrim(TFM)is a novel mesoionic pyrido[1,2-α]pyrimidinones insecticide,which acts on nicotinic acetylcholine receptors(n ACh Rs)and has no cross-resistance with other insecticides.Herein,we firstly developed...Triflumezopyrim(TFM)is a novel mesoionic pyrido[1,2-α]pyrimidinones insecticide,which acts on nicotinic acetylcholine receptors(n ACh Rs)and has no cross-resistance with other insecticides.Herein,we firstly developed a new continuous flow approach to synthesis 2-[3-(trifluoromethyl)phenyl]malonic acid,a key intermate of TFM,coupling with esterification,condensation,and hydrolysis.All three-step reactions were optimized and transformed into a continuous synthesis mode by three micro reaction units.Compared with the batch mode,the total reaction time and overall separation yield were improved from more than 12 h and 60%to 18 min and 73.38%,respectively.The solvent consumption and waste emission were significantly reduced,which also provides an eco-friendly and efficient potential tool for the development and production of mesoionic pyrido[1,2-α]pyrimidinones insecticide.展开更多
Cu/SiO2 catalysts prepared by the ammonia evaporation method were applied to hydrogenation of diethyl malonate to 1,3‐propanediol. The calcination temperature played an important role in the structural evolution and ...Cu/SiO2 catalysts prepared by the ammonia evaporation method were applied to hydrogenation of diethyl malonate to 1,3‐propanediol. The calcination temperature played an important role in the structural evolution and catalytic performance of the Cu/SiO2 catalysts, which were systematically characterized by N2 adsorption‐desorption, inductively coupled plasma‐atomic emission spectros‐copy, N2O chemisorption, X‐ray diffraction, Fourier transform infrared spectroscopy, H2 tempera‐ture‐programmed reduction, transmission electron microscopy, and X‐ray photoelectron spectros‐copy. When the Cu/SiO2 catalyst was calcined at 723 K, 90.7%conversion of diethyl malonate and 32.3%selectivity of 1,3‐propanediol were achieved. Compared with Cu/SiO2 catalysts calcined at other temperatures, the enhanced catalytic performance of the Cu/SiO2 catalyst calcined at 723 K can be attributed to better dispersion of copper species, larger cupreous surface area and greater amount of copper phyllosilicate, which results in a higher ratio of Cu＋/Cu0. The synergetic effect of Cu0 and Cu＋is suggested to be responsible for the optimum activity.展开更多
Based on the stability results of Radix hedysari extract, an unstable compound was extracted using acidic methanol and purified by rapid chromatographic methods successfully from Radix hedysari for the first time guid...Based on the stability results of Radix hedysari extract, an unstable compound was extracted using acidic methanol and purified by rapid chromatographic methods successfully from Radix hedysari for the first time guided by HPLC analysis. Its structure was identified as formononetin 7-O-β-D-（6＂-O-malonyl）-glucopyranoside by spectroscopic analyses.展开更多
Bennv Green和Russell Malone在2003年推出首张专辑《Jazz at the Bistro》后，这个钢琴和吉他爵十乐二重奏组合义在乐迷的期待中推出了《蓝鸟》(Bluebird)，这次推出的专辑依然由Telarc发行制作。许多人是在圣路易斯的“the Bistro”...Bennv Green和Russell Malone在2003年推出首张专辑《Jazz at the Bistro》后，这个钢琴和吉他爵十乐二重奏组合义在乐迷的期待中推出了《蓝鸟》(Bluebird)，这次推出的专辑依然由Telarc发行制作。许多人是在圣路易斯的“the Bistro”俱乐部里领略了Bennv Green和Russell Malone的出色表演。展开更多
In two experiments, the effects of succinate and NADH（reduced nicotinamide adenine dinucleotide） on metmyoglobin reductase activity and electron transport chain-linked metmyoglobin reduction were investigated and co...In two experiments, the effects of succinate and NADH（reduced nicotinamide adenine dinucleotide） on metmyoglobin reductase activity and electron transport chain-linked metmyoglobin reduction were investigated and compared. In experiment 1, metmyoglobin（MetMb）, substrate and inhibitors were incubated with mitochondria. Comparsion of the effects of succinate and NADH on MetMb reduction was investigated. The MetMb percentage in sample treated with 8 mol L-1 succinate decreased by about 69% after 3 h incubation, and the effect was inhibited by the addition of 10 mol L-1 electron transfer chain complex II inhibitor malonic acid; the MetMb percentage in samples treated with 2 mol L-1 NADH decreased by 56% and the effect was inhibited by the addition of 0.02 mol L-1 electron transport chain complex I inhibitor rotenone. These results indicated that electron transport chain played an important role in MetMb reduction. Both complex II and complex I take part in the MetMb reduction in mitochondria through different pathways. NADH-MetMb reduction system was less stable than succinateMetMb system. In experiment 2, the beef longissimus dorsi muscle was blended with different concentrations of succinate or NADH. Enhancing patties with higher concentration of succinate or NADH improved colour stability in vacuum packaged samples（P〈0.05）. These results verified that mitochondria electron transport chain is related to the MetMb reduction in meat system.展开更多
A new ternary complex [Ni（phen）（pmal）]·8H2O （phen = 1,10-phenanthroline, pmal^2- = phenethyl malonic acid） has been synthesized by the reaction of nickel acetate, phen and phenethyl malonic acid. Elemental ...A new ternary complex [Ni（phen）（pmal）]·8H2O （phen = 1,10-phenanthroline, pmal^2- = phenethyl malonic acid） has been synthesized by the reaction of nickel acetate, phen and phenethyl malonic acid. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. Crystal data for this complex： triclinic system, space group PI^-, a = 10.387（5）, b = 13.112（6）, c = 14.229（6） °A, α= 76.176（7）, β = 83.778（8）, γ = 71.770（6）°, C35H42N4O12Ni, Mr= 769.44, Z = 2, F（000） = 808, V = 1786.1°A^3, Dc = 1.431 g/cm^3,μ= 0.612 mm^-1, the final R = 0.0653 and wR = 0.1033 for 9379 （Rint = 0.0244） independent reflections and 4730 observed reflections （I〉 2σ（I））. Structural analysis shows that the coordination geometry of Ni（Ⅱ） is a distorted octahedron. A novel two-dimensional structure is constructed from （H2O）4 and （H2O）12 water clusters, and the complex forms a 3-D network supramolecular structure by hydrogen bonds and π-π stacking of neighboring phens.展开更多
Highly efficient Michael addition reactions of malonates to nitroalkenes catalyzed by novel chiral thioureas derived from optically pure BINOL and amino acids are reported. Various trans-nitroalkenes reacted with malo...Highly efficient Michael addition reactions of malonates to nitroalkenes catalyzed by novel chiral thioureas derived from optically pure BINOL and amino acids are reported. Various trans-nitroalkenes reacted with malonates affording the desired products in up to 95% yield with excellent enantioselectivities （up to 97% ee）.展开更多
The reaction of 4,4?-diaminodiphenylmethane (dadm), malonic acid (H2mal) and Cu(NO3)2 in aqueous solution results in a discrete binuclear Cu(II) macrocycle: [Cu(dadm)(mal)- (H2O)]22H2O. It crystallizes in monoclinic, ...The reaction of 4,4?-diaminodiphenylmethane (dadm), malonic acid (H2mal) and Cu(NO3)2 in aqueous solution results in a discrete binuclear Cu(II) macrocycle: [Cu(dadm)(mal)- (H2O)]22H2O. It crystallizes in monoclinic, space group P21/c with a = 15.231(3), b = 11.847(2), c = 9.801(2) ? b = 106.75(3)o, V = 1693.5(6) 3, Z = 2, C32H40Cu2N4O12, Mr = 799.76, Dc = 1.568 g/cm3, ?(MoKa) = 0.71073 ? = 1.325 mm-1, F(000) = 828, the final R = 0.0531 and wR = 0.1244 for 3421 observed reflections with I > 2s(I). Each Cu(II) is coordinated by two oxygen atoms from a mal ligand, two nitrogen atoms from two dadm ligands and a water oxygen atom to form a triangle bipyramidal motif. The title compound possesses a distorted macrocycle enclosed by dadm with approximate dimensions of 8.3 ??5.9 ?展开更多
Ionic liquids （ILs） based on 1,3-dialkylimidazolium and tetraalkylammonium cations were employed as a series of efficient, environmentally benign phase-transfer catalysts （PTCs） for the base-promoted monoalkylatio...Ionic liquids （ILs） based on 1,3-dialkylimidazolium and tetraalkylammonium cations were employed as a series of efficient, environmentally benign phase-transfer catalysts （PTCs） for the base-promoted monoalkylation of diethyl malonate. The influence of various heterogeneous bases on yields was studied. Good yields and high selectivity were obtained. Solvent-free, mild reaction condition, short reaction time, and easy purification were the merits of this method. The catalytic system （IL-hase） could also be recycled after the extraction of products with ether.展开更多
Two dinuclear compounds [Ln2（acetate）6（H2O）4]-4H2O （Ln=Tb（1）, Sm（2）） were obtained by the hydrothermal reaction of Ln2O3 with malonic acid at 150 ℃. Both compounds were characterized by elemental analyses, ...Two dinuclear compounds [Ln2（acetate）6（H2O）4]-4H2O （Ln=Tb（1）, Sm（2）） were obtained by the hydrothermal reaction of Ln2O3 with malonic acid at 150 ℃. Both compounds were characterized by elemental analyses, infrared spectra, and single crystal X-ray diffraction. The results showed that complexes 1 and 2 were isomorphous and crystallize in triclinic space group P 1. The coordination geometry around Ln（Ⅲ） ions in the complexes 1 and 2 was a distorted tricapped trigonal prism with a nine coordination. In the crystal, the molecular organization was further stabilized by well-defined weak hydrogen bonding interactions between the neutral dinuclear molecular units that led to the formation of a three-dimensional network. The fluorescence properties of the two complexes 1 and 2 in organic solvents were also studied. The results show that the ligand acetate favored energy transfer to the emitting energy level of Tb（Ⅲ） in complex 1. Some factors that influence the fluorescent intensity were also discussed in the article.展开更多
基金the National Key Research and Development Program of China(Nos.2023YFD1700303,2022YFD17800)National Natural Science Foundation of China(Nos.21878088,21476077)for financial support。
文摘Triflumezopyrim(TFM)is a novel mesoionic pyrido[1,2-α]pyrimidinones insecticide,which acts on nicotinic acetylcholine receptors(n ACh Rs)and has no cross-resistance with other insecticides.Herein,we firstly developed a new continuous flow approach to synthesis 2-[3-(trifluoromethyl)phenyl]malonic acid,a key intermate of TFM,coupling with esterification,condensation,and hydrolysis.All three-step reactions were optimized and transformed into a continuous synthesis mode by three micro reaction units.Compared with the batch mode,the total reaction time and overall separation yield were improved from more than 12 h and 60%to 18 min and 73.38%,respectively.The solvent consumption and waste emission were significantly reduced,which also provides an eco-friendly and efficient potential tool for the development and production of mesoionic pyrido[1,2-α]pyrimidinones insecticide.
文摘Cu/SiO2 catalysts prepared by the ammonia evaporation method were applied to hydrogenation of diethyl malonate to 1,3‐propanediol. The calcination temperature played an important role in the structural evolution and catalytic performance of the Cu/SiO2 catalysts, which were systematically characterized by N2 adsorption‐desorption, inductively coupled plasma‐atomic emission spectros‐copy, N2O chemisorption, X‐ray diffraction, Fourier transform infrared spectroscopy, H2 tempera‐ture‐programmed reduction, transmission electron microscopy, and X‐ray photoelectron spectros‐copy. When the Cu/SiO2 catalyst was calcined at 723 K, 90.7%conversion of diethyl malonate and 32.3%selectivity of 1,3‐propanediol were achieved. Compared with Cu/SiO2 catalysts calcined at other temperatures, the enhanced catalytic performance of the Cu/SiO2 catalyst calcined at 723 K can be attributed to better dispersion of copper species, larger cupreous surface area and greater amount of copper phyllosilicate, which results in a higher ratio of Cu＋/Cu0. The synergetic effect of Cu0 and Cu＋is suggested to be responsible for the optimum activity.
基金National Natural Science Foundation of China (Grant No.20432030 and 20872006).
文摘Based on the stability results of Radix hedysari extract, an unstable compound was extracted using acidic methanol and purified by rapid chromatographic methods successfully from Radix hedysari for the first time guided by HPLC analysis. Its structure was identified as formononetin 7-O-β-D-（6＂-O-malonyl）-glucopyranoside by spectroscopic analyses.
文摘Bennv Green和Russell Malone在2003年推出首张专辑《Jazz at the Bistro》后，这个钢琴和吉他爵十乐二重奏组合义在乐迷的期待中推出了《蓝鸟》(Bluebird)，这次推出的专辑依然由Telarc发行制作。许多人是在圣路易斯的“the Bistro”俱乐部里领略了Bennv Green和Russell Malone的出色表演。
基金the National Natural Science Foundation of China (31071624)
文摘In two experiments, the effects of succinate and NADH（reduced nicotinamide adenine dinucleotide） on metmyoglobin reductase activity and electron transport chain-linked metmyoglobin reduction were investigated and compared. In experiment 1, metmyoglobin（MetMb）, substrate and inhibitors were incubated with mitochondria. Comparsion of the effects of succinate and NADH on MetMb reduction was investigated. The MetMb percentage in sample treated with 8 mol L-1 succinate decreased by about 69% after 3 h incubation, and the effect was inhibited by the addition of 10 mol L-1 electron transfer chain complex II inhibitor malonic acid; the MetMb percentage in samples treated with 2 mol L-1 NADH decreased by 56% and the effect was inhibited by the addition of 0.02 mol L-1 electron transport chain complex I inhibitor rotenone. These results indicated that electron transport chain played an important role in MetMb reduction. Both complex II and complex I take part in the MetMb reduction in mitochondria through different pathways. NADH-MetMb reduction system was less stable than succinateMetMb system. In experiment 2, the beef longissimus dorsi muscle was blended with different concentrations of succinate or NADH. Enhancing patties with higher concentration of succinate or NADH improved colour stability in vacuum packaged samples（P〈0.05）. These results verified that mitochondria electron transport chain is related to the MetMb reduction in meat system.
基金Project supported by the Natural Science Foundation of Liaoning Province (No. 20052014), the Foundation of Education Committee of Liaoning Province (2004C021) and the Ph. D. Programs Foundation of Shenyang Institute of Chemical Technology
文摘A new ternary complex [Ni（phen）（pmal）]·8H2O （phen = 1,10-phenanthroline, pmal^2- = phenethyl malonic acid） has been synthesized by the reaction of nickel acetate, phen and phenethyl malonic acid. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. Crystal data for this complex： triclinic system, space group PI^-, a = 10.387（5）, b = 13.112（6）, c = 14.229（6） °A, α= 76.176（7）, β = 83.778（8）, γ = 71.770（6）°, C35H42N4O12Ni, Mr= 769.44, Z = 2, F（000） = 808, V = 1786.1°A^3, Dc = 1.431 g/cm^3,μ= 0.612 mm^-1, the final R = 0.0653 and wR = 0.1033 for 9379 （Rint = 0.0244） independent reflections and 4730 observed reflections （I〉 2σ（I））. Structural analysis shows that the coordination geometry of Ni（Ⅱ） is a distorted octahedron. A novel two-dimensional structure is constructed from （H2O）4 and （H2O）12 water clusters, and the complex forms a 3-D network supramolecular structure by hydrogen bonds and π-π stacking of neighboring phens.
基金support from Natural Science Foundation of China(No.20772097)Sichuan Provincial Science Foundation for Outstanding Youth(No.05ZQ026-008)Key Project of the Education Department of Sichuan Province(No.2006A081).
文摘Highly efficient Michael addition reactions of malonates to nitroalkenes catalyzed by novel chiral thioureas derived from optically pure BINOL and amino acids are reported. Various trans-nitroalkenes reacted with malonates affording the desired products in up to 95% yield with excellent enantioselectivities （up to 97% ee）.
文摘The reaction of 4,4?-diaminodiphenylmethane (dadm), malonic acid (H2mal) and Cu(NO3)2 in aqueous solution results in a discrete binuclear Cu(II) macrocycle: [Cu(dadm)(mal)- (H2O)]22H2O. It crystallizes in monoclinic, space group P21/c with a = 15.231(3), b = 11.847(2), c = 9.801(2) ? b = 106.75(3)o, V = 1693.5(6) 3, Z = 2, C32H40Cu2N4O12, Mr = 799.76, Dc = 1.568 g/cm3, ?(MoKa) = 0.71073 ? = 1.325 mm-1, F(000) = 828, the final R = 0.0531 and wR = 0.1244 for 3421 observed reflections with I > 2s(I). Each Cu(II) is coordinated by two oxygen atoms from a mal ligand, two nitrogen atoms from two dadm ligands and a water oxygen atom to form a triangle bipyramidal motif. The title compound possesses a distorted macrocycle enclosed by dadm with approximate dimensions of 8.3 ??5.9 ?
文摘Ionic liquids （ILs） based on 1,3-dialkylimidazolium and tetraalkylammonium cations were employed as a series of efficient, environmentally benign phase-transfer catalysts （PTCs） for the base-promoted monoalkylation of diethyl malonate. The influence of various heterogeneous bases on yields was studied. Good yields and high selectivity were obtained. Solvent-free, mild reaction condition, short reaction time, and easy purification were the merits of this method. The catalytic system （IL-hase） could also be recycled after the extraction of products with ether.
基金the National Natural Science Foundation of China (20772037)the Natural Science Foundation of Guangdong Province (06025033)
文摘Two dinuclear compounds [Ln2（acetate）6（H2O）4]-4H2O （Ln=Tb（1）, Sm（2）） were obtained by the hydrothermal reaction of Ln2O3 with malonic acid at 150 ℃. Both compounds were characterized by elemental analyses, infrared spectra, and single crystal X-ray diffraction. The results showed that complexes 1 and 2 were isomorphous and crystallize in triclinic space group P 1. The coordination geometry around Ln（Ⅲ） ions in the complexes 1 and 2 was a distorted tricapped trigonal prism with a nine coordination. In the crystal, the molecular organization was further stabilized by well-defined weak hydrogen bonding interactions between the neutral dinuclear molecular units that led to the formation of a three-dimensional network. The fluorescence properties of the two complexes 1 and 2 in organic solvents were also studied. The results show that the ligand acetate favored energy transfer to the emitting energy level of Tb（Ⅲ） in complex 1. Some factors that influence the fluorescent intensity were also discussed in the article.
