Because of the great virtue of Heck reaction and one-pot reaction,Recently it attract many attention that how to synthesis indoles by this two methods,and has gained many progress.But It is still a problem that how to...Because of the great virtue of Heck reaction and one-pot reaction,Recently it attract many attention that how to synthesis indoles by this two methods,and has gained many progress.But It is still a problem that how to synthesis indoles through one-pot reaction with o-haloaniline and open-chain ketone.Here,for the first time,we synthesized 3-ethoxycarbonyl-2-methylindole through one-pot Heck reaction with o-bromoaniline and open-chain ketone ethyl acetoacetate.Farther work is in progress.展开更多
Pd/LaxPbyMnOz, Pd/C, Pd/molecular sieve and Pd-heteropoly acid catalysts for direct synthesis of diphenyl carbonate (DPC) by heterogeneous catalytic reaction were compared and the results of DPC synthesis indicated th...Pd/LaxPbyMnOz, Pd/C, Pd/molecular sieve and Pd-heteropoly acid catalysts for direct synthesis of diphenyl carbonate (DPC) by heterogeneous catalytic reaction were compared and the results of DPC synthesis indicated that the catalyst Pd/LaxPbyMnOz had higher activity. The Pd/LaxPbyMnOz catalyst and the support was characterized by XRD, SEM and TEM, the main phase was Lao.szPbo.asMnOa and the average diameter could be about 25.4nm. The optimuna conditions for synthesis of DPC with Pd/LasPbyMnOz were determined by orthogonal experiments and the experimental results showed that reaction temperature was the first factor of effect on the selectivity and yield of DPC, and the concentration of O2 in gas phase also had significant effect on selectivity of DPC. The optimum reaction conditions were catalyst/phenol mass ratio l to 50, pressure 4.5MPa, volume concentration of O2 25%, reaction temperature 60℃ and reaction time 4 h. The maximum yield and average selectivity could reach 13% and 97% respectively in the batch operation.展开更多
The magnetic perovskite-supported palladium catalysts Pd/Lal_xPbxMnO3 (x = 0.2-0.7) were prepared and used for the oxidative carbonylation of phenol to diphenyl carbonate. The synthesized catalysts were characterize...The magnetic perovskite-supported palladium catalysts Pd/Lal_xPbxMnO3 (x = 0.2-0.7) were prepared and used for the oxidative carbonylation of phenol to diphenyl carbonate. The synthesized catalysts were characterized by the X-ray diffraction (XRD), surface area measurement BET, vibration sample magnetometer (VSM) and tem- perature-programmed reduction (TPR). The experimental results demonstrated that the magnetic Pd/La1-xPbxMnO3 (x = 0.4-0.5) obtain relative better catalytic activity. It can be explained by higher concentration of oxygen vacan- cies, larger amount and better mobility of lattice oxygen of their support. Furthermore, these samples possess suffi- cient saturated magnetization. Thus, Pd/La1-xPbxMnO3 (x = 0.4-0.5) may be suitable for operation in the magneti- cally stabilized bed reactor.展开更多
Methyl 3-hydroxypropanoate was synthesized via hydroesterification of ethylene oxide with CO in the presence of dicobalt octacarbonyl catalyst and methanol solvent. The catalyst exhibited high catalytic activity. The ...Methyl 3-hydroxypropanoate was synthesized via hydroesterification of ethylene oxide with CO in the presence of dicobalt octacarbonyl catalyst and methanol solvent. The catalyst exhibited high catalytic activity. The effect of reaction temperature, CO pressure, methanol dosage, catalyst dosage and reaction time on catalytic reaction was investigated. The test results revealed that this reaction was greatly affected by reaction temperature, but it was not significantly affected by the CO pressure, the methanol dosage, the catalyst dosage and the reaction time. Under the optimal conditions, the conversion of ethylene oxide was equal to 92.24%, while the selectivity and yield of methyl 3-hydroxypropanoate reached 88.99% and 84.35%, respectively.展开更多
文摘Because of the great virtue of Heck reaction and one-pot reaction,Recently it attract many attention that how to synthesis indoles by this two methods,and has gained many progress.But It is still a problem that how to synthesis indoles through one-pot reaction with o-haloaniline and open-chain ketone.Here,for the first time,we synthesized 3-ethoxycarbonyl-2-methylindole through one-pot Heck reaction with o-bromoaniline and open-chain ketone ethyl acetoacetate.Farther work is in progress.
基金National Natural Science Foundation of China(No.20076036Tianjin University C1 National Laboratory Project
文摘Pd/LaxPbyMnOz, Pd/C, Pd/molecular sieve and Pd-heteropoly acid catalysts for direct synthesis of diphenyl carbonate (DPC) by heterogeneous catalytic reaction were compared and the results of DPC synthesis indicated that the catalyst Pd/LaxPbyMnOz had higher activity. The Pd/LaxPbyMnOz catalyst and the support was characterized by XRD, SEM and TEM, the main phase was Lao.szPbo.asMnOa and the average diameter could be about 25.4nm. The optimuna conditions for synthesis of DPC with Pd/LasPbyMnOz were determined by orthogonal experiments and the experimental results showed that reaction temperature was the first factor of effect on the selectivity and yield of DPC, and the concentration of O2 in gas phase also had significant effect on selectivity of DPC. The optimum reaction conditions were catalyst/phenol mass ratio l to 50, pressure 4.5MPa, volume concentration of O2 25%, reaction temperature 60℃ and reaction time 4 h. The maximum yield and average selectivity could reach 13% and 97% respectively in the batch operation.
基金Supported by the Key Program of National Natural Science Foundation of China(20936003)the Foundation for Innovation Research Groups of the Natural Science Foundation of Hubei Province(2008CDA009)
文摘The magnetic perovskite-supported palladium catalysts Pd/Lal_xPbxMnO3 (x = 0.2-0.7) were prepared and used for the oxidative carbonylation of phenol to diphenyl carbonate. The synthesized catalysts were characterized by the X-ray diffraction (XRD), surface area measurement BET, vibration sample magnetometer (VSM) and tem- perature-programmed reduction (TPR). The experimental results demonstrated that the magnetic Pd/La1-xPbxMnO3 (x = 0.4-0.5) obtain relative better catalytic activity. It can be explained by higher concentration of oxygen vacan- cies, larger amount and better mobility of lattice oxygen of their support. Furthermore, these samples possess suffi- cient saturated magnetization. Thus, Pd/La1-xPbxMnO3 (x = 0.4-0.5) may be suitable for operation in the magneti- cally stabilized bed reactor.
基金supported by the Guangdong Province Natural Science Foundation (No. 10152500002000019)the Maoming City Science and Technology Planning Project (NO.2008024)
文摘Methyl 3-hydroxypropanoate was synthesized via hydroesterification of ethylene oxide with CO in the presence of dicobalt octacarbonyl catalyst and methanol solvent. The catalyst exhibited high catalytic activity. The effect of reaction temperature, CO pressure, methanol dosage, catalyst dosage and reaction time on catalytic reaction was investigated. The test results revealed that this reaction was greatly affected by reaction temperature, but it was not significantly affected by the CO pressure, the methanol dosage, the catalyst dosage and the reaction time. Under the optimal conditions, the conversion of ethylene oxide was equal to 92.24%, while the selectivity and yield of methyl 3-hydroxypropanoate reached 88.99% and 84.35%, respectively.