The photo-induced vapor-phase decomposition of dimethyl ether was investigated on Pt metals deposited on pure and N-doped TiO2. Infrared spectroscopic measurements revealed that adsorption of dimethyl ether on TiO2 sa...The photo-induced vapor-phase decomposition of dimethyl ether was investigated on Pt metals deposited on pure and N-doped TiO2. Infrared spectroscopic measurements revealed that adsorption of dimethyl ether on TiO2 samples underwent partial dissociation to methoxy species. Illumination of the (CH3)2O-TiO2 and (CH3)2O-M/TiO2 systems led to the conversion of methoxy into adsorbed formate. In the case of metal-promoted TiO2 catalysts, CO bonded to the metals was also detected. Pure titania exhibited a very little photoactivity. Deposition of Pt metals on TiO2 markedly enhanced the extent of photocatalytic decomposition of dimethyl ether to give H2 and CO2 as the major products. A small amount of CO and methyl formate was also identified in the products. The most active metal was the Rh followed by Pd, Ir, Pt and Ru. When the bandgap of TiO2 was lowered by N-doping, the photocatalytic activity of metal/TiO2 catalysts appreciably increased. The effect of metals was explained by a better separation of charge carriers induced by illumination and by enhanced electronic interaction between metal nanoparticles and TiO2.展开更多
Five novel bis—(N—alkyl—N,N—dimethyl ammoni(?)n)polyethyleneglyool ether salts prepared by our previously reported proced(?)e show high catalytic efficiency in the condensation of 1,4—diacetyl— 2,5—piperazinedi...Five novel bis—(N—alkyl—N,N—dimethyl ammoni(?)n)polyethyleneglyool ether salts prepared by our previously reported proced(?)e show high catalytic efficiency in the condensation of 1,4—diacetyl— 2,5—piperazinedione and aldehydes at both higher and lower temperature even in lower concentration.They al so show catalytic selectivity at lower temperature.展开更多
Synthesis of methyl N-phenyl carbamate from dimethyl carbonate and 1,3-diphenyl urea was investigated under atmospheric pressure. The results showed that homogenous catalyst sodium methoxide had the excellent activity...Synthesis of methyl N-phenyl carbamate from dimethyl carbonate and 1,3-diphenyl urea was investigated under atmospheric pressure. The results showed that homogenous catalyst sodium methoxide had the excellent activity to efficiently catalyze the synthesis of methyl N-phenyl carbamate under atmospheric pressure.展开更多
The title compound 4-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）-N- （pyridin-2-yl） thiazol-2-amine was synthesized by reacting 2-bromo-1-（7-methoxy-2,2-dime- thyl-2,3-dihydrobenzofuran-5-yl）ethanone with...The title compound 4-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）-N- （pyridin-2-yl） thiazol-2-amine was synthesized by reacting 2-bromo-1-（7-methoxy-2,2-dime- thyl-2,3-dihydrobenzofuran-5-yl）ethanone with 1-（pyridine-2-yl）thiourea, and its crystal was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, chiral space group C2 with a = 18.1328（14）, b = 5.5969（5）, c = 19.2195（15） A, β= 115.5420（10）°, V= 1759.9（2）A3, Z = 4, F（000） = 744, C19H19N3O2S, Mr= 353.43, Dc= 1.334 g/cm3, S = 1.15, μ = 0.201 mm-1, the final R = 0.035 and wR = 0.111 for 2307 observed reflections （I 〉 2σ（I））. The Flack parameter is -0.03（10）. The preliminary bioassay result indicated that the title compound exhibits strong insecticidal activity （93.75% mortality） against Mythimna separate at the concentration of 1.000 g/L.展开更多
β-Cyclodextrin( β-CyD) is cyclic oligosaccharide of a glucopyranose, containing a relatively hydrophobic central cavity and hydrophilic outer surface. However, the usefulness of β-CyD is limited owing to its low aq...β-Cyclodextrin( β-CyD) is cyclic oligosaccharide of a glucopyranose, containing a relatively hydrophobic central cavity and hydrophilic outer surface. However, the usefulness of β-CyD is limited owing to its low aqueous solubility whereas we found that its apparent high solubility was evident in some injectable solvents including 2-pyrrolidone(PYR), Nmethyl pyrrolidone(NMP) and dimethyl sulfoxide(DMSO). Therefore, in the present study, the physicochemical properties of the 30–60% w/w β-CyD in PYR, NMP and DMSO were investigated such as viscosity, water resistant, matrix formation rate and syringeability. The higher the concentration of β-CyD resulted in the increased viscosity and the higher force and energy of syringeability. β-CyD in PYR gave the highest viscosity which contributed to the lowest syringeability while β-CyD in DMSO exhibited the highest syringeability. The β-CyD in DMSO and NMP exhibited the higher rate of matrix formation. β-CyD in PYR showed the highest water resistant for phase separation while β-CyD in NMP gave the faster de-mixing rate compared to that from PYR. The difference in physicochemical properties of β-CyD dried ppts studied by scanning electron microscope(SEM), differential scanning calorimetry(DSC), X-ray diffraction(XRD), Fourier-transform infrared spectroscopy(FT-IR) and thermogravimetric analysis(TGA) revealed that there was partial complexation of β-CyD with respective solvents. Both solution and precipitate characteristic properties will be useful for using β-CyD in further investigation as matrix material dissolved in the injectable vehicles as the in situ forming gel for periodontitis treatment.展开更多
The title compound N,N＇-bis（5,5-dimethyl-2-phospha-2-thio-1,3-dioxan-2-yl） ethylene diamine （DPTDEDA, C12H26N2O4P2S2） was synthesized by the reaction of neopentyl glycol, phosphorus thio-chloride and 1,2-ethylene...The title compound N,N＇-bis（5,5-dimethyl-2-phospha-2-thio-1,3-dioxan-2-yl） ethylene diamine （DPTDEDA, C12H26N2O4P2S2） was synthesized by the reaction of neopentyl glycol, phosphorus thio-chloride and 1,2-ethylenediamine, and characterized by elemental analysis, IR and ^1H NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction analysis and the thermal property was analyzed by TG analysis. The crystal structure belongs to monoclinic, space group P21/c, with a = 14.557（16）, b = 11.299（12）, c = 12.163（13）A,β = 98.707（19）^o, Dc = 1.305 g/cm^3, Z = 4, γ = 0.71073A,μ（MoKa） = 0.447 mm^-1, Mr = 388.41, V = 1977（4）A3, F（000） = 824, S = 1.107, the final R = 0.0478 and wR = 0.0810 for 1738 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the crystal structure is centrosymmetrically distributed through 1,2-ethylenediamine to join two distorted six-membered rings. The weak N-H…S interactions are observed and link the molecules into sheets. TG analysis shows that the title compound has good thermal stability and char-forming capability, which are required for an excellent intumescent fire retardant.展开更多
以间苯二胺为原料,与酰化剂甲酸反应制得中间体N,N'-二甲酰基间苯二胺,再以NABH4-I2为还原剂合成得到产品N,N'-二甲基间苯二胺,对合成工艺进行了优化,并分析了还原机理,化合物的结构经IR,1 H NMR和MS分析确定.该法原料易得,反...以间苯二胺为原料,与酰化剂甲酸反应制得中间体N,N'-二甲酰基间苯二胺,再以NABH4-I2为还原剂合成得到产品N,N'-二甲基间苯二胺,对合成工艺进行了优化,并分析了还原机理,化合物的结构经IR,1 H NMR和MS分析确定.该法原料易得,反应条件要求低,收率高且成本更低.展开更多
文摘The photo-induced vapor-phase decomposition of dimethyl ether was investigated on Pt metals deposited on pure and N-doped TiO2. Infrared spectroscopic measurements revealed that adsorption of dimethyl ether on TiO2 samples underwent partial dissociation to methoxy species. Illumination of the (CH3)2O-TiO2 and (CH3)2O-M/TiO2 systems led to the conversion of methoxy into adsorbed formate. In the case of metal-promoted TiO2 catalysts, CO bonded to the metals was also detected. Pure titania exhibited a very little photoactivity. Deposition of Pt metals on TiO2 markedly enhanced the extent of photocatalytic decomposition of dimethyl ether to give H2 and CO2 as the major products. A small amount of CO and methyl formate was also identified in the products. The most active metal was the Rh followed by Pd, Ir, Pt and Ru. When the bandgap of TiO2 was lowered by N-doping, the photocatalytic activity of metal/TiO2 catalysts appreciably increased. The effect of metals was explained by a better separation of charge carriers induced by illumination and by enhanced electronic interaction between metal nanoparticles and TiO2.
文摘Five novel bis—(N—alkyl—N,N—dimethyl ammoni(?)n)polyethyleneglyool ether salts prepared by our previously reported proced(?)e show high catalytic efficiency in the condensation of 1,4—diacetyl— 2,5—piperazinedione and aldehydes at both higher and lower temperature even in lower concentration.They al so show catalytic selectivity at lower temperature.
文摘Synthesis of methyl N-phenyl carbamate from dimethyl carbonate and 1,3-diphenyl urea was investigated under atmospheric pressure. The results showed that homogenous catalyst sodium methoxide had the excellent activity to efficiently catalyze the synthesis of methyl N-phenyl carbamate under atmospheric pressure.
基金Project supported by the National Technology R&D Program (No. 2011 BAE06B01)
文摘The title compound 4-（7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl）-N- （pyridin-2-yl） thiazol-2-amine was synthesized by reacting 2-bromo-1-（7-methoxy-2,2-dime- thyl-2,3-dihydrobenzofuran-5-yl）ethanone with 1-（pyridine-2-yl）thiourea, and its crystal was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, chiral space group C2 with a = 18.1328（14）, b = 5.5969（5）, c = 19.2195（15） A, β= 115.5420（10）°, V= 1759.9（2）A3, Z = 4, F（000） = 744, C19H19N3O2S, Mr= 353.43, Dc= 1.334 g/cm3, S = 1.15, μ = 0.201 mm-1, the final R = 0.035 and wR = 0.111 for 2307 observed reflections （I 〉 2σ（I））. The Flack parameter is -0.03（10）. The preliminary bioassay result indicated that the title compound exhibits strong insecticidal activity （93.75% mortality） against Mythimna separate at the concentration of 1.000 g/L.
文摘β-Cyclodextrin( β-CyD) is cyclic oligosaccharide of a glucopyranose, containing a relatively hydrophobic central cavity and hydrophilic outer surface. However, the usefulness of β-CyD is limited owing to its low aqueous solubility whereas we found that its apparent high solubility was evident in some injectable solvents including 2-pyrrolidone(PYR), Nmethyl pyrrolidone(NMP) and dimethyl sulfoxide(DMSO). Therefore, in the present study, the physicochemical properties of the 30–60% w/w β-CyD in PYR, NMP and DMSO were investigated such as viscosity, water resistant, matrix formation rate and syringeability. The higher the concentration of β-CyD resulted in the increased viscosity and the higher force and energy of syringeability. β-CyD in PYR gave the highest viscosity which contributed to the lowest syringeability while β-CyD in DMSO exhibited the highest syringeability. The β-CyD in DMSO and NMP exhibited the higher rate of matrix formation. β-CyD in PYR showed the highest water resistant for phase separation while β-CyD in NMP gave the faster de-mixing rate compared to that from PYR. The difference in physicochemical properties of β-CyD dried ppts studied by scanning electron microscope(SEM), differential scanning calorimetry(DSC), X-ray diffraction(XRD), Fourier-transform infrared spectroscopy(FT-IR) and thermogravimetric analysis(TGA) revealed that there was partial complexation of β-CyD with respective solvents. Both solution and precipitate characteristic properties will be useful for using β-CyD in further investigation as matrix material dissolved in the injectable vehicles as the in situ forming gel for periodontitis treatment.
基金This work was supported by the China Petroleum & Chemical Science and Technology Foundation (No. 205026) the Tianjin Science and Technology Plan Foundation (No. 06TXTJJC14400)
文摘The title compound N,N＇-bis（5,5-dimethyl-2-phospha-2-thio-1,3-dioxan-2-yl） ethylene diamine （DPTDEDA, C12H26N2O4P2S2） was synthesized by the reaction of neopentyl glycol, phosphorus thio-chloride and 1,2-ethylenediamine, and characterized by elemental analysis, IR and ^1H NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction analysis and the thermal property was analyzed by TG analysis. The crystal structure belongs to monoclinic, space group P21/c, with a = 14.557（16）, b = 11.299（12）, c = 12.163（13）A,β = 98.707（19）^o, Dc = 1.305 g/cm^3, Z = 4, γ = 0.71073A,μ（MoKa） = 0.447 mm^-1, Mr = 388.41, V = 1977（4）A3, F（000） = 824, S = 1.107, the final R = 0.0478 and wR = 0.0810 for 1738 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the crystal structure is centrosymmetrically distributed through 1,2-ethylenediamine to join two distorted six-membered rings. The weak N-H…S interactions are observed and link the molecules into sheets. TG analysis shows that the title compound has good thermal stability and char-forming capability, which are required for an excellent intumescent fire retardant.
