In order to improve the yield and reduce the cost in the synthesis of antitumor drug vismodegib the key intermediates are prepared and the Negishi reaction step is examined.The effects of different molar ratios of rea...In order to improve the yield and reduce the cost in the synthesis of antitumor drug vismodegib the key intermediates are prepared and the Negishi reaction step is examined.The effects of different molar ratios of reactants dosages of catalyst and time for refluxing are investigated by using single factor tests.The results demonstrate that when the molar ratios of 2-bromopyridine 2-chloro-N-4-chloro-3-iodophenyl -4-methylsulfonyl benzamide zinc chloride n-butyllithium and tetrakis triphenyl phosphine palladium are changed to 1.0∶0.5∶1.5∶1.1∶0.05 and the mixture is refluxed for 24 h the production yield is improved to 72%.This reaction condition significantly enhances the synthetic efficiency avoids consuming excessive raw materials/catalysts and meanwhile prevents a prolonged reaction time.The optimization of the proportion of reactants and the heating time is proved to be important for the efficiency and economy in cross-coupling reaction to synthesize vismodegib.展开更多
In this paper, an efficient methodology for synthesizing the indirect work exchange networks(WEN) considering isothermal process and adiabatic process respectively based on transshipment model is first proposed. In co...In this paper, an efficient methodology for synthesizing the indirect work exchange networks(WEN) considering isothermal process and adiabatic process respectively based on transshipment model is first proposed. In contrast with superstructure method, the transshipment model is easier to obtain the minimum utility consumption taken as the objective function and more convenient for us to attain the optimal network configuration for further minimizing the number of units. Different from division of temperature intervals in heat exchange networks,different pressure intervals are gained according to the maximum compression/expansion ratio in consideration of operating principles of indirect work exchangers and the characteristics of no pressure constraints for stream matches. The presented approach for WEN synthesis is a linear programming model applied to the isothermal process, but for indirect work exchange networks with adiabatic process, a nonlinear programming model needs establishing. Additionally, temperatures should be regarded as decision variables limited to the range between inlet and outlet temperatures in each sub-network. The constructed transshipment model can be solved first to get the minimum utility consumption and further to determine the minimum number of units by merging the adjacent pressure intervals on the basis of the proposed merging methods, which is proved to be effective through exergy analysis at the level of units structures. Finally, two cases are calculated to confirm it is dramatically feasible and effective that the optimal WEN configuration can be gained by the proposed method.展开更多
A novel bead form of ploymer of high sorption capacity for urea were obtained by the reaction of glutaric dialdehyde wigh chitosan dispersed in acetic acid solution. The sorption capacity reached  ̄ 82.0 mg / g sorbe...A novel bead form of ploymer of high sorption capacity for urea were obtained by the reaction of glutaric dialdehyde wigh chitosan dispersed in acetic acid solution. The sorption capacity reached  ̄ 82.0 mg / g sorbent at 37℃ and pH 7.4 The concentration of urea in the buffer solution was 1300 mg/ L. The sorption of urea was related to the degree of crosslinking of the sorbent, concentration ofurea, ionic strength and temperature.展开更多
A highly crosslinked, monodispersed polystyrene(PS) particle was prepared by a seeded batch dispersion polymerization with a monomer absorption method. Prior to polymerization, 1,9 lam monodispersed PS seed particle...A highly crosslinked, monodispersed polystyrene(PS) particle was prepared by a seeded batch dispersion polymerization with a monomer absorption method. Prior to polymerization, 1,9 lam monodispersed PS seed particles were treated under an optimum condition of monomer absorption. The effects of divinylbenzebe(DVB) concentration and polymerization temperature were examined for styrene(in PS seed)/styrene(in the second stage) mass ratio of 1:1 in the medium range of EtOH/water mass ratio of 100/0-80/20 and 2.3 μm uniform crosslinked PS particles containing 15%-20% (mass fraction) DVB were prepared at 60-70 ℃. The results show that monomer absorption before the second stage of polymerization is more effective to prepare highly crosslinked monodispersed PS particles.展开更多
A concept of potential crosslinking agent was introduced into the synthesizing process of highly oil-absorptive resin that is traditionally prepared by single chemical crosslinking.The resin was heated after manufactu...A concept of potential crosslinking agent was introduced into the synthesizing process of highly oil-absorptive resin that is traditionally prepared by single chemical crosslinking.The resin was heated after manufactured to obtain three-dimension network structure.The effects of potential crosslinking agent and the crosslinking conditions on the absorptive properties of resin were studied.The results showed that hydroxyl ethylacrylate got satisfied results,and the resin with it had good oil absorbency and oil retention.展开更多
基金The National Basic Research Program of China(973Program)(No.2011CB933503)China Postdoctoral Science Foundation(No.2013M541592)
文摘In order to improve the yield and reduce the cost in the synthesis of antitumor drug vismodegib the key intermediates are prepared and the Negishi reaction step is examined.The effects of different molar ratios of reactants dosages of catalyst and time for refluxing are investigated by using single factor tests.The results demonstrate that when the molar ratios of 2-bromopyridine 2-chloro-N-4-chloro-3-iodophenyl -4-methylsulfonyl benzamide zinc chloride n-butyllithium and tetrakis triphenyl phosphine palladium are changed to 1.0∶0.5∶1.5∶1.1∶0.05 and the mixture is refluxed for 24 h the production yield is improved to 72%.This reaction condition significantly enhances the synthetic efficiency avoids consuming excessive raw materials/catalysts and meanwhile prevents a prolonged reaction time.The optimization of the proportion of reactants and the heating time is proved to be important for the efficiency and economy in cross-coupling reaction to synthesize vismodegib.
基金Supported by the National Natural Science Foundation of China(21576036 and 21776035)
文摘In this paper, an efficient methodology for synthesizing the indirect work exchange networks(WEN) considering isothermal process and adiabatic process respectively based on transshipment model is first proposed. In contrast with superstructure method, the transshipment model is easier to obtain the minimum utility consumption taken as the objective function and more convenient for us to attain the optimal network configuration for further minimizing the number of units. Different from division of temperature intervals in heat exchange networks,different pressure intervals are gained according to the maximum compression/expansion ratio in consideration of operating principles of indirect work exchangers and the characteristics of no pressure constraints for stream matches. The presented approach for WEN synthesis is a linear programming model applied to the isothermal process, but for indirect work exchange networks with adiabatic process, a nonlinear programming model needs establishing. Additionally, temperatures should be regarded as decision variables limited to the range between inlet and outlet temperatures in each sub-network. The constructed transshipment model can be solved first to get the minimum utility consumption and further to determine the minimum number of units by merging the adjacent pressure intervals on the basis of the proposed merging methods, which is proved to be effective through exergy analysis at the level of units structures. Finally, two cases are calculated to confirm it is dramatically feasible and effective that the optimal WEN configuration can be gained by the proposed method.
文摘A novel bead form of ploymer of high sorption capacity for urea were obtained by the reaction of glutaric dialdehyde wigh chitosan dispersed in acetic acid solution. The sorption capacity reached  ̄ 82.0 mg / g sorbent at 37℃ and pH 7.4 The concentration of urea in the buffer solution was 1300 mg/ L. The sorption of urea was related to the degree of crosslinking of the sorbent, concentration ofurea, ionic strength and temperature.
基金the second stage of BK21 program for supporting a fellowship
文摘A highly crosslinked, monodispersed polystyrene(PS) particle was prepared by a seeded batch dispersion polymerization with a monomer absorption method. Prior to polymerization, 1,9 lam monodispersed PS seed particles were treated under an optimum condition of monomer absorption. The effects of divinylbenzebe(DVB) concentration and polymerization temperature were examined for styrene(in PS seed)/styrene(in the second stage) mass ratio of 1:1 in the medium range of EtOH/water mass ratio of 100/0-80/20 and 2.3 μm uniform crosslinked PS particles containing 15%-20% (mass fraction) DVB were prepared at 60-70 ℃. The results show that monomer absorption before the second stage of polymerization is more effective to prepare highly crosslinked monodispersed PS particles.
文摘A concept of potential crosslinking agent was introduced into the synthesizing process of highly oil-absorptive resin that is traditionally prepared by single chemical crosslinking.The resin was heated after manufactured to obtain three-dimension network structure.The effects of potential crosslinking agent and the crosslinking conditions on the absorptive properties of resin were studied.The results showed that hydroxyl ethylacrylate got satisfied results,and the resin with it had good oil absorbency and oil retention.