A novel chiral phosphine-triazine ligand was synthesized from chiral α-phenylethylamine through a three-step procedure. In a model reaction of Pd-catalyzed allylic alkylation of rac-1,3-diphenylprop-2-en-1-y1 pivalat...A novel chiral phosphine-triazine ligand was synthesized from chiral α-phenylethylamine through a three-step procedure. In a model reaction of Pd-catalyzed allylic alkylation of rac-1,3-diphenylprop-2-en-1-y1 pivalate with dimethyl malonate, good enantioselectivity (90% e.e.) was obtained by using this ligand.展开更多
A mixed stationary phase of modified β-cyclodextrin, 2,6-di-O-butyl-3-O-butyryl-β-cyclodextrin (phase A), and SE-54 (phase B) was used for enantiomeric separation of α-phenylethylami-ne, o,m,p-methyl and o,m,p-meth...A mixed stationary phase of modified β-cyclodextrin, 2,6-di-O-butyl-3-O-butyryl-β-cyclodextrin (phase A), and SE-54 (phase B) was used for enantiomeric separation of α-phenylethylami-ne, o,m,p-methyl and o,m,p-methoxy-substituted analogs. The composition of mixed phase was selected by comparison of each calculated amin(= (γm,i+1)/(γm,i))> the relative retention values of the most adjacent peaks, and γm,last, the relative retention values of the last eluting peak at each preselected ratio. Values of γm,i,α calculated by derived equations were in good agreement with the experimental results obtained with two specified mixed phases. All solutes investigated were almost baseline separated at a predicted composition of phase A and phase B in a single run within 18 minutes.展开更多
1 Results It has been reported that crystalline form racemates can be resoluted by various methods[1],but for optical resolution of liquid form racemates,the method is limited in chromatograph.So chiral compounds cann...1 Results It has been reported that crystalline form racemates can be resoluted by various methods[1],but for optical resolution of liquid form racemates,the method is limited in chromatograph.So chiral compounds cannot be obtained on large scale by such method.In our previous paper,(+)-3-chloro-1,2-propanediol has been obtained by optical resolution of its racemata (liquid) with a chiral biopolymer,casein[2].展开更多
Unexpected dealkylation of Bischler-Napieralski cyclization of 2-(3,4-dimethoxy-2- nitro-phenyl)-N-[2-(3,4-dimethoxyphenyl) ethyl]-N-[(S)-1-phenyl-ethyl] acetamide 3 was reported. The electronic effect of the substitu...Unexpected dealkylation of Bischler-Napieralski cyclization of 2-(3,4-dimethoxy-2- nitro-phenyl)-N-[2-(3,4-dimethoxyphenyl) ethyl]-N-[(S)-1-phenyl-ethyl] acetamide 3 was reported. The electronic effect of the substituent at 2-position of C ring was also discussed.展开更多
2-Phenylethylamine(2-PEA)is one of the main ingredients for stimulants.Therefore,it is necessary to limit its use and illegal trade by conveniently detecting 2-PEA vapour.Here,a QCM based 2-PEA gas sensor was construc...2-Phenylethylamine(2-PEA)is one of the main ingredients for stimulants.Therefore,it is necessary to limit its use and illegal trade by conveniently detecting 2-PEA vapour.Here,a QCM based 2-PEA gas sensor was constructed by using aldehyde functionalized mesoporous carbon(FDU-15-CHO)as sensing materials designed according to Schiff base adsorption role.The 2D hexagonal mesoporous structures of the sensing material have been confirmed by small-angle X-ray diffraction(SXRD),transmission electron microscopy(TEM),and N2adsorption-desorption isotherms.The covalent grafting of aldehyde group onto the FDU-15 was confirmed by Fourier transform infrared spectroscopy(FT-IR).FDU-15-CHO based Quartz Crystal Microbalance(QCM)sensor shows better sensitivity to 2-PEA than its parent FDU-15.Besides,the detection limit of FDU-15-CHO based sensor can reach down to 1 ppm,and its selectivity and reproducibility are satisfactory.The high concentrations of active sites in the mesopores of FDU-15 are believed to facilitate 2-PEA adsorption,and thus the presence of the-CHO group leading to sensitive and selective response,which is verified by Gaussian simulation.展开更多
文摘A novel chiral phosphine-triazine ligand was synthesized from chiral α-phenylethylamine through a three-step procedure. In a model reaction of Pd-catalyzed allylic alkylation of rac-1,3-diphenylprop-2-en-1-y1 pivalate with dimethyl malonate, good enantioselectivity (90% e.e.) was obtained by using this ligand.
基金Project supported by the National Natural Science Foundation of China.
文摘A mixed stationary phase of modified β-cyclodextrin, 2,6-di-O-butyl-3-O-butyryl-β-cyclodextrin (phase A), and SE-54 (phase B) was used for enantiomeric separation of α-phenylethylami-ne, o,m,p-methyl and o,m,p-methoxy-substituted analogs. The composition of mixed phase was selected by comparison of each calculated amin(= (γm,i+1)/(γm,i))> the relative retention values of the most adjacent peaks, and γm,last, the relative retention values of the last eluting peak at each preselected ratio. Values of γm,i,α calculated by derived equations were in good agreement with the experimental results obtained with two specified mixed phases. All solutes investigated were almost baseline separated at a predicted composition of phase A and phase B in a single run within 18 minutes.
文摘1 Results It has been reported that crystalline form racemates can be resoluted by various methods[1],but for optical resolution of liquid form racemates,the method is limited in chromatograph.So chiral compounds cannot be obtained on large scale by such method.In our previous paper,(+)-3-chloro-1,2-propanediol has been obtained by optical resolution of its racemata (liquid) with a chiral biopolymer,casein[2].
文摘Unexpected dealkylation of Bischler-Napieralski cyclization of 2-(3,4-dimethoxy-2- nitro-phenyl)-N-[2-(3,4-dimethoxyphenyl) ethyl]-N-[(S)-1-phenyl-ethyl] acetamide 3 was reported. The electronic effect of the substituent at 2-position of C ring was also discussed.
基金the National Nature Science Foundation of China(No.61527818)the Shanghai Municipal Education Commission(Peak Discipline Construction Program)for their generous support。
文摘2-Phenylethylamine(2-PEA)is one of the main ingredients for stimulants.Therefore,it is necessary to limit its use and illegal trade by conveniently detecting 2-PEA vapour.Here,a QCM based 2-PEA gas sensor was constructed by using aldehyde functionalized mesoporous carbon(FDU-15-CHO)as sensing materials designed according to Schiff base adsorption role.The 2D hexagonal mesoporous structures of the sensing material have been confirmed by small-angle X-ray diffraction(SXRD),transmission electron microscopy(TEM),and N2adsorption-desorption isotherms.The covalent grafting of aldehyde group onto the FDU-15 was confirmed by Fourier transform infrared spectroscopy(FT-IR).FDU-15-CHO based Quartz Crystal Microbalance(QCM)sensor shows better sensitivity to 2-PEA than its parent FDU-15.Besides,the detection limit of FDU-15-CHO based sensor can reach down to 1 ppm,and its selectivity and reproducibility are satisfactory.The high concentrations of active sites in the mesopores of FDU-15 are believed to facilitate 2-PEA adsorption,and thus the presence of the-CHO group leading to sensitive and selective response,which is verified by Gaussian simulation.