In this paper, sodium cobalt tetracarbonyl （NaCo（CO）4） was synthesized by using sodium dithionite and zinc powder as the reduction system and cobalt hexahydrate acetate as the precursor in the presence of methanol...In this paper, sodium cobalt tetracarbonyl （NaCo（CO）4） was synthesized by using sodium dithionite and zinc powder as the reduction system and cobalt hexahydrate acetate as the precursor in the presence of methanol solvent. Methyl 3-hydroxypropionate was synthesized via hydroesterification of ethylene oxide （EO） catalyzed by NaCo（CO）4. The influencing factors on the reaction results were discussed, including the different ligands, the molar ratio of solvent and ethylene oxide, the reaction temperature, the reaction time, and the reaction pressure. An optimal catalytic system was obtained by using 3-hydroxypyridine as the ligoad under reaction conditions covering a reaction temperature 65 ℃, a reaction time of 7 h, a reaction pressure of 6 MPa, and a methoaol/EO molar ratio of 3：2. Under the optimal conditions, the conversion of ethylene oxide was equal to 97.86%, while the selectivity and yield of methyl 3-hydroxypropionate reached 88.19% and 86.30%, respectively. Finally, the reaction mechanism of hydroesterification of ethylene oxide catalyzed by NaCo（CO）4 was proposed.展开更多
The title compounds(Me_2SiSiMe_2)(η-RC_3H_3)Fe(CO)(μ-CO)_2(R:H(1a),Me(1b))were prepared by heating a solution of RC_(?)H_4(Me_2SiSiMe_2)C_5H_4R and Fe(CO)_5 in xylene at reflux.(1a)and(1b)can convert into their isom...The title compounds(Me_2SiSiMe_2)(η-RC_3H_3)Fe(CO)(μ-CO)_2(R:H(1a),Me(1b))were prepared by heating a solution of RC_(?)H_4(Me_2SiSiMe_2)C_5H_4R and Fe(CO)_5 in xylene at reflux.(1a)and(1b)can convert into their isomers Me_2Si(η-RC_3H_3)Fe(CO)_2(?)2(R:H(2a), Me(2b))under the reaction conditions.The crystal and molecular structures of(1a),(2a) and(2b)were determined by X-ray diffraction.展开更多
Sodium tetracarbonyl cobaltate was prepared by reaction of CO with CoCl2 inCH3OH, using Urushibara-Cobalt (U-Co) as activator and characterized by IR spectrometry-The optimum conditions were: Co(from U-Co)/CoCl2=0. 6;...Sodium tetracarbonyl cobaltate was prepared by reaction of CO with CoCl2 inCH3OH, using Urushibara-Cobalt (U-Co) as activator and characterized by IR spectrometry-The optimum conditions were: Co(from U-Co)/CoCl2=0. 6; 30 ℃; 0. 1 MPa of CO. Theconvertion of CoCl2 in 3 h of reaction was 96%. The convertion of benzyl chloride to pheny-lacetic acid using the Na[Co(CO)4] as catalyst was about 90% at 50℃ and 0. 1 MPa of CO.展开更多
基金supported by the Guangdong Province Natural Science Foundation (No.10152500002000019)the Maoming City Science and Technology Planning Project(No.2014069)
文摘In this paper, sodium cobalt tetracarbonyl （NaCo（CO）4） was synthesized by using sodium dithionite and zinc powder as the reduction system and cobalt hexahydrate acetate as the precursor in the presence of methanol solvent. Methyl 3-hydroxypropionate was synthesized via hydroesterification of ethylene oxide （EO） catalyzed by NaCo（CO）4. The influencing factors on the reaction results were discussed, including the different ligands, the molar ratio of solvent and ethylene oxide, the reaction temperature, the reaction time, and the reaction pressure. An optimal catalytic system was obtained by using 3-hydroxypyridine as the ligoad under reaction conditions covering a reaction temperature 65 ℃, a reaction time of 7 h, a reaction pressure of 6 MPa, and a methoaol/EO molar ratio of 3：2. Under the optimal conditions, the conversion of ethylene oxide was equal to 97.86%, while the selectivity and yield of methyl 3-hydroxypropionate reached 88.19% and 86.30%, respectively. Finally, the reaction mechanism of hydroesterification of ethylene oxide catalyzed by NaCo（CO）4 was proposed.
文摘The title compounds(Me_2SiSiMe_2)(η-RC_3H_3)Fe(CO)(μ-CO)_2(R:H(1a),Me(1b))were prepared by heating a solution of RC_(?)H_4(Me_2SiSiMe_2)C_5H_4R and Fe(CO)_5 in xylene at reflux.(1a)and(1b)can convert into their isomers Me_2Si(η-RC_3H_3)Fe(CO)_2(?)2(R:H(2a), Me(2b))under the reaction conditions.The crystal and molecular structures of(1a),(2a) and(2b)were determined by X-ray diffraction.
文摘Sodium tetracarbonyl cobaltate was prepared by reaction of CO with CoCl2 inCH3OH, using Urushibara-Cobalt (U-Co) as activator and characterized by IR spectrometry-The optimum conditions were: Co(from U-Co)/CoCl2=0. 6; 30 ℃; 0. 1 MPa of CO. Theconvertion of CoCl2 in 3 h of reaction was 96%. The convertion of benzyl chloride to pheny-lacetic acid using the Na[Co(CO)4] as catalyst was about 90% at 50℃ and 0. 1 MPa of CO.
