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Versatile MOF-derived cobalt catalyst for the reductive amination

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Science China Materials 2017年第12期60卷 1269-1271页

作者： Haihong Wu Chaoren Shen chungu xia Lin He State Key Laboratory for Oxo Synthesis and Selective Oxidation Suzhou Research Institute of LICP Lanzhou Institute of Chemical Physics (LICP) Chinese Academy of Sciences Lanzhou 730000 China University of Chinese Academy of Sciences Beijing 100049 China

The tunable metal center and the tailorable organic linker of metal-organic framework(MOF)make the characteristic of ultrahigh porosity,controllable pore size,crystalline nature and highly-ordered structures[1].Since its emergence[2,3],it represents one of the most celebrated functional *** to the rich diversity of MOF family,a vast of important applications including the storage of gas,recognition of molecules as well as

关键词： DABCO Co NH MOF TPA

Biosynthesis of poly-3-hydroxybutyrate with a high molecular weight by methanotroph from methane and methanol

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Journal of Natural Gas Chemistry 2008年第1期17卷 103-109页

作者： Yingxin Zhang Jiaying Xin Linlin Chen Hao Song chungu xia State Key Laboratory for Oxo Synthesis ＆ Selective Oxidation Lanzhou Institute of Chemical Physics Chinese Academy of Sciences Lanzhou 730000 China College of Food Engineering Harbin University of Commerce Harbin 150076 China Graduate University of Chinese Academy of Sciences Beijing 10039 China

Poly-3-hydroxybutyrate （PHB） can be produced by various species of bacteria. Among the possible carbon sources, both methane and methanol could be a suitable substrate for the production of PHB. Methane is cheap and plentiful not only as natural gas, but also as biogas. Methanol can also maintain methanotrophic activity in some conditions. The methanotrophic strain Methylosinus trichosporium IMV3011 can accumulate PHB with methane and methanol in a brief nonsterile process. Liquid methanol （0.1%） was added to improve the oxidization of methane. The studies were carried out using shake flasks. Cultivation was performed in two stages： a continuous growth phase and a PHB accumulation phase under the conditions short of essential nutrients （ammonium, nitrate, phosphorus, copper, iron （Ⅲ）, magnesium or ethylenediamine tetraacetate （EDTA）） in batch culture. It was found that the most suitable growth time for the cell is 144 h. Then an optimized culture condition for second stage was determined, in which the PHB concentration could be much increased to 0.6 g/L. In order to increase PHB content, citric acid was added as an inhibitor of tricarboxylic acid cycle （TCA）. It was found that citric acid is favorable for the PHB accumulation, and the PHB yield was increased to 40% （w/w） from the initial yield of 12% （w/w） after nutrient deficiency cultivation. The PHB produced is of very high quality with molecular weight up to 1.5 × 10^6Da.

关键词： poly-3-hydroxybutyrate methanotrophs methane methanol cultivation biosynthesis high molecular weight

A novel manganese(Ⅲ)-peroxo complex bearing a proline-derived pentadentate aminobenzimidazole ligand

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Chinese Chemical Letters 2018年第12期29卷 1869-1871页

作者： Junyi Du Chengxia Miao chungu xia Wei Sun State Key Laboratory for Oxo Synthesis and Selective Oxidation Suzhou Research Institute of LICPLanzhou Institute of Chemical Physics(LICP)Chinese Academy of SciencesLanzhou 730000China University of Chinese Academy of Sciences Beijing 100049China

Manganese(Ⅲ)-peroxo complexes are invoked as key intermediates in the enzymatic cycles of Mncontaining enzymes, and the synthesis of reactive manganese(Ⅲ)-peroxo complexes with rationally designed ligand has been of great interest in the communities of bioinorganic and biomimetic ***, we designed a novel pentadentate aminobenzimidazole ligand and obtained its manganese(Ⅱ)complex, which was successfully applied in the synthesis of a reactive manganese(Ⅲ)-peroxo complex by treatment with hydrogen peroxide in the presence of triethylamine. The manganese(Ⅲ)-peroxo complex was well characterized with various spectroscopic techniques, including ultraviolet-visible(UV-vis)spectrophotometry, coldspray ionization time-of-flight mass spectrometry(CSI-TOF MS), and continuous wave electron paramagnetic resonance(CW-EPR) spectroscopy. Besides, its reactivity in aldehyde deformylation was investigated, demonstrating second-order kinetics in the reaction with 2-phenylpropionaldehyde and affording acetophenone as the sole product.

关键词： Enzyme models Manganese Manganese(Ⅲ)-peroxo complex Aldehyde deformylation Kinetics

Magnetically Separable and Versatile Pd/Fe3O4 Catalyst for Efficient Suzuki Cross-Coupling Reaction and Selective Hydrogenation of Nitroarenes

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Chinese Journal of Chemistry 2011年第3期29卷 525-530页

作者： Zhang, Rongzhao Liu, Jianming Li, Fuwei Wang, Shoufeng xia, chungu Sun, Wei State Key Laboratory for Oxo Synthesis and Selective Oxidation Lanzhou Institute of Chemical Physics Chinese Academy of Sciences Lanzhou Gansu 730000 China Graduate School of the Chinese Academy of Sciences Beijing 100039 China

Magnetic nanoparticle-supported Pd/Fe3O4 was readily prepared and proved to be versatile catalyst for efficient Suzuki cross-coupling reaction, and the reduction of nitroarenes under mild conditions （balloon H2 pressure and room temperature）. The catalyst could be conveniently recovered and reused several times with sustained catalytic activity.

关键词： nanoparticles Fe3O4 supported catalyst Suzuki coupling reaction reduction

Photoinduced Transition-Metal-Free Alkynylation of Alkyl Pinacol Boronates

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CCS Chemistry 2021年第6期3卷 1718-1728页

作者： Dunfa Shi chungu xia Chao Liu State Key Laboratory for Oxo Synthesis and Selective Oxidation CAS Key Laboratory of Chemistry of Northwestern Plant ResourcesSuzhou Research InstituteLanzhou Institute of Chemical PhysicsChinese Academy of SciencesLanzhou 730000 University of Chinese Academy of Sciences Beijing 100049

An unprecedented visible-light-induced transitionmetal-free alkynylation of alkyl pinacol boronates has been demonstrated with alkynyl phenylsulfones as the alkynylation reagents and 4CzIPN as the organic *** sodium methoxide(NaOMe)or sodium hydroxide(NaOH)was used as the Lewis base togeneratephotoactivetetra-coordinatedboron *** functional groupswerewell *** selective monoalkynylation of diboronates was achieved to keep one boryl group in the product for potential further *** trapping experiments and electron paramagnetic resonance(EPR)analysis confirmed the generation of alkyl radical intermediate.

关键词： organoboron photocatalysis C-C coupling radical synthetic methods

NiCo/Al_(2)O_(3)nanocatalysts for the synthesis of 5-amino-1-pentanol and 1,5-pentanediol from biomass-derived 2-hydroxytetrahydropyran

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Green Chemical Engineering 2024年第1期5卷 119-131页

作者： Jian Yang Jia Zhang Enrico Benassi Xuemei Li Hailong Liu Weiguo Fang Junying Tian chungu xia Zhiwei Huang State Key Laboratory for Oxo Synthesis and Selective Oxidation Lanzhou Institute of Chemical PhysicsChinese Academy of SciencesLanzhou730000China School of Petrochemical Engineering Lanzhou University of TechnologyLanzhou730050China Novosibirsk State University Novosibirsk630090Russia University of Chinese Academy of Sciences Beijing100049China

Al_(2)O_(3)-supported monometallic Ni,Co,and bimetallic Ni-Co nanocatalysts originated from layered double hydroxide precursors were synthesized by co-precipitation method,and used for the synthesis of useful 5-amino-1-pentanol(5-AP)and 1,5-pentanediol(1,5-PD)by reductive amination(RA)or direct hydrogenation of biofurfuralderived 2-hydroxytetrahydropyran(2-HTHP),*** both reactions,the yield of the target products decreased monotonously with the increasing amounts of Co in the NiCo/Al_(2)O_(3)catalysts,owing probably to the replacement of highly reactive Ni by Co component with inferior hydrogenation activity at the low reaction temperature of 60℃.However,the incorporation of Co could improve the reducibility of the NiCo/Al_(2)O_(3)bimetallic catalysts and promote the reaction stability of the catalysts,especially for Ni_(2)Co1/Al_(2)O_(3),in both reactions with over 180 h *** of the catalysts before and after the reaction showed that the incorporating Co could inhibit the sintering of metal particles and hinder the surface oxidation of the more reactive Ni0species,thanks to the formation of Ni-Co alloy in the bimetallic ***-based modeling of the reaction mechanisms is also performed,supporting the reaction pathway proposed previously and also the much higher activity of Ni in the RA of 2-HTHP as compared with Co.

关键词： NiCo bimetallic catalysts Layered double hydroxide Reductive amination Amino alcohol Quantum chemical calculations

Chemical equilibrium controlled synthesis of polyoxymethylene dimethyl ethers over sulfated titania

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Journal of Energy Chemistry 2015年第2期24卷 239-244页

作者： Huaju Li Huanling Song Feng Zhao Liwei Chen chungu xia Laboratory for Nano-Catalytic Material & Technology Division of Advanced Nano?materials Suzhou Institute of Nano-Tech and Nano-BionicsChinese Academy of Sciences State Key Laboratory for Oxo Synthesis and Selective Oxidation Lanzhou Institute of Chemical Physics Chinese Academy of Sciences i-Lab Suzhou Institute of Nano-Tech and Nano-Bionics Chinese Academy of Sciences

The chemical equilibrium and reaction kinetic behavior in the synthesis of polyoxymethylene dimethyl ethers （DMMn） were investigated over sulfated titania in order to reveal the decisive factor controlling the reaction. The results showed that the molar ratio of adjacent DMMn products in equilibrium solution had the same value, which depended absolutely on the reaction temperature. Meanwhile, the reactions had the same DMMn products distributions under varied reaction conditions. The equilibrium constants of the related step-wise reactions for DMMn formation were equal, which were calculated based on the bulk compositions of the reaction solution. And thus, the selectivity to DMMn was mainly controlled by the chemical equilibrium, i.e., thermodynamic control. In brief, the present results provide some guidance for future synthesis of DMMn.

关键词： polyoxymethylene dimethyl ethers sulfated titania chemical equilibrium reaction kinetic molar ratio

Intermediate formation enabled regioselective access to amide in the Pd-catalyzed reductive aminocarbonylation of olefin with nitroarene

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Chinese Journal of Catalysis 2020年第7期41卷 1152-1160页

作者： Li Yang Lijun Shi chungu xia Fuwei Li State Key Laboratory for Oxo Synthesis and Selective Oxidation Suzhou Research Institute of LICPLanzhou Institute of Chemical Physics(LICP)Chinese Academy of SciencesLanzhou 730000GansuChina

An efficient route for the palladium-catalyzed reductive aminocarbonylation of olefins with nitroarenes was developed using carbon monoxide(CO)as both reductant and carbonyl source,which enables facile access to amides with excellent regioselectivity and broad substrate *** is found that the counter anions of the Pd catalyst precursors significantly affect the reaction chemoselectivity and amide *** amides were mainly obtained with K2PdCl4 as the metal catalyst,and phosphine ligands had no influence on the regioselectivity but affected the catalytic ***,phosphine ligands had significant effects on aminocarbonylation regioselectivity when Pd(CH3CN)4(OTf)2 was used;monodentate phosphines tended to form branched amides,and bidentate phosphines mainly formed linear *** experiments,primary kinetic studies,and control reactions with all possible N-species reduced from nitroarene indicated that the catalytic synthesis of branched and linear amides produced nitrene(further converted to enamide)and aniline,respectively,different from the previous ligand-controlled regioselective synthesis of amides via the aminocarbonylation of olefins with ***,the proposed synthesis route could be applied in the synthesis of gram-scale propanil under mild conditions.

关键词： Nitroarenes Amides N-intermediate Aminocarbonylation Regioselectivity

Enantioselective epoxidation of olefins with hydrogen peroxide catalyzed by bioinspired aminopyridine manganese complexes derived from L-proline

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Chinese Journal of Catalysis 2018年第9期39卷 1463-1469页

作者： Wenfang Wang Qiangsheng Sun chungu xia Wei Sun State Key Laboratory for Oxo Synthesis and Selective Oxidation Lanzhou Institute of Chemical Physics Chinese Academy of Sciences Lanzhou 730000 Gansu China University of Chinese Academy of Sciences Beijing 100049 China

Three chiral aminopyridine ligands derived from L-proline were prepared. Careful evaluation of the corresponding aminopyridine manganese complexes in asymmetric epoxidation of olefins revealed a broad substrate scope in the presence of 0.2 mol% manganese complex and 0.5 equiv. 2,2-dimethylbutyric acid, with aqueous hydrogen peroxide as an oxidant. A variety of olefins including styrenes, chromenes, and cinnamamides were transformed successfully into the target epoxides with moderate to excellent enantioselectivity（yield up to 95%, ee up to 99%）.

关键词： Aminopyridine ligand Manganese Asymmetricep oxidation Hydrogenperoxide Olefin