The production of Ph3Sn–O–SBA-15(Ph3Sn SBA)was achieved by heating triphenyltin chloride and SBA-15in N-methylpyrrolidone at 190°C for 5 h using triethylamine as a catalyst.The composition,structure,and surface...The production of Ph3Sn–O–SBA-15(Ph3Sn SBA)was achieved by heating triphenyltin chloride and SBA-15in N-methylpyrrolidone at 190°C for 5 h using triethylamine as a catalyst.The composition,structure,and surface physical and chemical properties of Ph3Sn SBA were characterized using inductively coupled plasma-atomic emission spectroscopy(ICP-AES),13C,119Sn and29Si solid-state nuclear magnetic resonance(NMR)spectroscopy in situ pyridine infrared spectroscopy(Py-IR),N2adsorption–desorption isotherms,X-ray diffraction(XRD)and transmission electron microscopy(TEM).The results of ICP-AES and organic elemental analysis showed that the grafting yield of Sn was 17%(by mass)for Ph3Sn SBA.The elemental analysis and solid-state NMR results for Ph3Sn SBA were consistent with grafting of triphenyltin on SBA-15.The N2adsorption–desorption,XRD and TEM analyses showed that Ph3Sn SBA retained an ordered hexagonal mesoporous structure,resulting in decreases in the surface area,pore size and mesopore volume,and an increase in acidity as compared with SBA-15.The Hammett acidity function(H0)value and the number of acid sites for Ph3Sn SBA,obtained by the Hammett methods,were 2.77–3.30 and 2.07 mmol·g-1,respectively.The Friedel–Crafts acylation of toluene and acetic anhydride over Ph3Sn SBA was investigated.The yield of methylacetophenone(MAP)and the selectivity for 4-methylacetophenone(PMAP)were 79.56%and 97.12%,respectively,when the conditions were n(toluene):n(anhydride)=2.0:1.0 with 6%(by mass)catalyst,and heating under reflux for 5 h.The PMAP selectivity still reached 93.11%when Ph3Sn SBA was used for the fifth time under the same reaction conditions.展开更多
Hydroxy-phenyl)-5-(2-methyl-phenyl)-6-ethoxycarbonyl-cyclohexen-2-one has been synthesized and characterized by elemental analysis, IR, UV, H NMR and MS, and its crystal 1 structure was determined by X-ray single-crys...Hydroxy-phenyl)-5-(2-methyl-phenyl)-6-ethoxycarbonyl-cyclohexen-2-one has been synthesized and characterized by elemental analysis, IR, UV, H NMR and MS, and its crystal 1 structure was determined by X-ray single-crystal diffraction method. The crystal belongs to the monoclinic system, space group P21/c with a = 14.6298(13), b = 5.8623(5), c = 22.255(2) ?, β = 105.855(2)o, V = 1836.0(3) ?3, Mr = 350.40, Z = 4, Dc = 1.268 g/cm3, F(000) = 744, μ(MoKα) = 0.086 mm-1, R = 0.0680 and wR = 0.1498. The crystal analysis results show that the cyclohexene unit of the title compound has a quasi-chair conformation, and a centrosymmetric dimer with a 16-membered ring is produced by the intermolecular hydrogen bonds.展开更多
基金Supported by the National Science Foundation of Heilongjiang Province(B201010)the Education Department of Heilongjiang Province(12511595)
文摘The production of Ph3Sn–O–SBA-15(Ph3Sn SBA)was achieved by heating triphenyltin chloride and SBA-15in N-methylpyrrolidone at 190°C for 5 h using triethylamine as a catalyst.The composition,structure,and surface physical and chemical properties of Ph3Sn SBA were characterized using inductively coupled plasma-atomic emission spectroscopy(ICP-AES),13C,119Sn and29Si solid-state nuclear magnetic resonance(NMR)spectroscopy in situ pyridine infrared spectroscopy(Py-IR),N2adsorption–desorption isotherms,X-ray diffraction(XRD)and transmission electron microscopy(TEM).The results of ICP-AES and organic elemental analysis showed that the grafting yield of Sn was 17%(by mass)for Ph3Sn SBA.The elemental analysis and solid-state NMR results for Ph3Sn SBA were consistent with grafting of triphenyltin on SBA-15.The N2adsorption–desorption,XRD and TEM analyses showed that Ph3Sn SBA retained an ordered hexagonal mesoporous structure,resulting in decreases in the surface area,pore size and mesopore volume,and an increase in acidity as compared with SBA-15.The Hammett acidity function(H0)value and the number of acid sites for Ph3Sn SBA,obtained by the Hammett methods,were 2.77–3.30 and 2.07 mmol·g-1,respectively.The Friedel–Crafts acylation of toluene and acetic anhydride over Ph3Sn SBA was investigated.The yield of methylacetophenone(MAP)and the selectivity for 4-methylacetophenone(PMAP)were 79.56%and 97.12%,respectively,when the conditions were n(toluene):n(anhydride)=2.0:1.0 with 6%(by mass)catalyst,and heating under reflux for 5 h.The PMAP selectivity still reached 93.11%when Ph3Sn SBA was used for the fifth time under the same reaction conditions.
基金This work was financially supported by the Education Committee of Hunan Province (02C465)Hunan Provincial Key Discipline and Hunan Provincial General College Leader of Learning
文摘Hydroxy-phenyl)-5-(2-methyl-phenyl)-6-ethoxycarbonyl-cyclohexen-2-one has been synthesized and characterized by elemental analysis, IR, UV, H NMR and MS, and its crystal 1 structure was determined by X-ray single-crystal diffraction method. The crystal belongs to the monoclinic system, space group P21/c with a = 14.6298(13), b = 5.8623(5), c = 22.255(2) ?, β = 105.855(2)o, V = 1836.0(3) ?3, Mr = 350.40, Z = 4, Dc = 1.268 g/cm3, F(000) = 744, μ(MoKα) = 0.086 mm-1, R = 0.0680 and wR = 0.1498. The crystal analysis results show that the cyclohexene unit of the title compound has a quasi-chair conformation, and a centrosymmetric dimer with a 16-membered ring is produced by the intermolecular hydrogen bonds.
