Nine indole alkaloids and one aromatic amine were isolated from Evodia rutaecarpa Benth. Their structures were identified as evodiamine(1),rutaecarpine(2),formyldihydrorutaecarpine(3),goshuyuamide I(4),evodiamide(5)...Nine indole alkaloids and one aromatic amine were isolated from Evodia rutaecarpa Benth. Their structures were identified as evodiamine(1),rutaecarpine(2),formyldihydrorutaecarpine(3),goshuyuamide I(4),evodiamide(5),hydroxyevodiamine(6),β carboline(7),1,2,3,4 tetrahydro 1 oxo β carboline(8),dehydroevodiamine(9)and N methylanthranylamide(10).Compound 8 was a new natural product. Compound 7 was for the first time isolated from Evodia.展开更多
The title compound (C_ 24H_ 40Cl_6O_ 16V_3, M_r = 950.08) was synthesized from the reaction of VCl_3 and NaO_2CEt in CHCl_3 and THF. The crystal structure has been determined by X-ray single-crystal diffraction ana...The title compound (C_ 24H_ 40Cl_6O_ 16V_3, M_r = 950.08) was synthesized from the reaction of VCl_3 and NaO_2CEt in CHCl_3 and THF. The crystal structure has been determined by X-ray single-crystal diffraction analysis. It crystallizes in monoclinic space group C2/c with a = 12.5768(4), b= 16.5601(4), c = 19.3574(7) , β = 99.879(1)°, V = 3971.3(2)3, D_c = 1.589 g/cm3, μ= 1.157 mm -1, F(000)=1932, Z=4, R = 0.055, wR = 0.1539 (I2σ(I)). This compound has an unusual coplanar V_3O core with a C_2 axis passing through O(1), V(1), O(10): one V-μ_3O is short (1.628 ), the other two are longer (2.381 ). It was characterized by IR, 1H NMR, and EPR spectra. It was unstable and the decomposition process of this compound was studied using IR spectroscopy.展开更多
The title compound [Ni(bipy)3][(-oxo)Fe2Cl6] (bipy = 2, 2?bispyridine) was synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group P2l/c with unit c...The title compound [Ni(bipy)3][(-oxo)Fe2Cl6] (bipy = 2, 2?bispyridine) was synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group P2l/c with unit cell parameters: a = 9.7085(7),b = 26.409(2), c = 14.014(1) ,?= 100.237(3), V = 3535.9(2) 3,Z = 4,C30H24Cl6Fe2N6NiO,Mr = 867.66, Dc = 1.630 g/cm3,F(000) = 1744, (MoK? = 1.824 mm-1, the final R = 0.0394 and wR = 0.0475 for 2750 observed reflections with I ≥ 2(I). The title compound contains cation of [Ni(bipy)3]2+ and anion of [(-oxo)Fe2Cl6] 2- which consists of two [FeCl3] fragments connected by an oxo bridge with the bond distances of Fe(2)O(1) 1.752(2) and Fe(1)O(1) 1.763(2) , and the bond angle of Fe(2)O(1)Fe(1) 148.6(2)? In the [Fe2(-oxo)Cl6]2- complex, the two iron(Ⅲ) centers exhibit a tetrahedral coordination with the distorted tetrahedron formed by three Cl atoms and one oxo bridge.展开更多
The single crystals of the title quaternary compound were synthesized by solid state reaction at 950℃ from SmOBr-V-NH_4Cl system.It crystallized in monoclinic system,space group C2/M with cell dimmensions of a=1.3255...The single crystals of the title quaternary compound were synthesized by solid state reaction at 950℃ from SmOBr-V-NH_4Cl system.It crystallized in monoclinic system,space group C2/M with cell dimmensions of a=1.3255(2) nm.b=0. 5588(5) nm, c=1.0942(5) nm;β=100.48(2)°;Γ=0.797(1) nm3; Z=2; Dc= 5.50 g/cm3 ; F(000) = 1190; μ(MoKα)=176.82cm-1.The final R and Rw for 1430 reflections with I>3.00 σ(I) were 0.071 and0.085 respectively.The Sm atoms are 8-coordinated.the V atoms have octahedral coordination environment and the Si atoms are tetrahedral.The structure of the title compound is built from vanadium octahedra layers and samarium-vanadium-silicate slabs.展开更多
A novel polyester containing glycolic acid(GA)and 2 hydro 2 oxo 1,3,2 dioxaphosphorinane(TMP)was prepared by ring opening polymerization.The composition and the structure of the titled polymer were investigated by 1...A novel polyester containing glycolic acid(GA)and 2 hydro 2 oxo 1,3,2 dioxaphosphorinane(TMP)was prepared by ring opening polymerization.The composition and the structure of the titled polymer were investigated by 1H NMR, 13 C NMR,FT IR,EA,and VPO.The influence of time on total conversion and molecular weight was also studied.展开更多
The reaction mechanism of OXO(X=Cl, Br) with H(2\%S\%) was studied theoretically by using the B3LYP/6-311+G(3df, 3pd) and the high-level electron-correlation QCISD(T)/6-311+G ** at single-point. The results show that ...The reaction mechanism of OXO(X=Cl, Br) with H(2\%S\%) was studied theoretically by using the B3LYP/6-311+G(3df, 3pd) and the high-level electron-correlation QCISD(T)/6-311+G ** at single-point. The results show that the mechanism for the title reaction involves three channels, from which OH+XO, HO 2+X and HX+O 2 products could be obtained, respectively. Therefore, the channel to yield the products OH+XO is the dominant one in agreement with the experiments.展开更多
Mesoporous zirconium oxo phosphate-sulfate was synthesized by hydrothermal method with hexadecyltrithylammonium bromide(CTAB)as the template and with zirconium nitrate or zirconium oxychloride as zirconium source.The ...Mesoporous zirconium oxo phosphate-sulfate was synthesized by hydrothermal method with hexadecyltrithylammonium bromide(CTAB)as the template and with zirconium nitrate or zirconium oxychloride as zirconium source.The optimum two-stage process was established, ^(31)P MAS NMR showed that the states of phosphate species were changed with further postsynthesis treatment by sulfate acid. The transformations of the structures at different temperatures from room temperature to 1173 K were investigated by XRD. ...展开更多
o-Carboxybenzaldehyde (1)and acetone gave the Claisen-Schmidt condensation product, which readily cyclizes on acidification to give 1-oxo-3-acetonyl-dihydrobenzo [c]furan(4)in 68% yield. Other methyl ketones behaved s...o-Carboxybenzaldehyde (1)and acetone gave the Claisen-Schmidt condensation product, which readily cyclizes on acidification to give 1-oxo-3-acetonyl-dihydrobenzo [c]furan(4)in 68% yield. Other methyl ketones behaved similarly.展开更多
A variety of gold（Ⅲ） adducts having a-ligated oxygen-donor ligands have been prepared from [Au（ppy）Cl2]（ppy.phenylpyridine）（1） either by partial or total replacement of the chloride ions. The new species comp...A variety of gold（Ⅲ） adducts having a-ligated oxygen-donor ligands have been prepared from [Au（ppy）Cl2]（ppy.phenylpyridine）（1） either by partial or total replacement of the chloride ions. The new species comprise hydroxo-[Au（ppy）（OH）Cl]（2）, and [Au（ppy）（OH）2]（3）, oxo-[Au2（ppy）2（μ-O）2]（4）, acetate-[Au（ppy）（O2CMe2）] （5）, and alkoxo complexes-[Au（ppy）（OR）Cl]（6, 7） and [Au（ppy）（OR）2]（8--10）（R=Me, 6 and 8; Et, 7 and 9; Pr, 10）. The dihydroxo and the oxo complexes can be interconverted by refluxing the former in anhydrous THF and the latter in water. The hydroxides 2 and 3 and the acetato complex 5 undergo σ-ligand metathesis in ROH solution（R=Me, Et or Pr） to give the corresponding alkoxides.展开更多
The dihydric dithioketenes 3a-c obtained by 1,2-addition of methallyl Grignard reagent to bis(alkylthio)methylidene derivative ofdimedone 2a-c wewr converted to the cycloaromatization product 4 assisted by boron trifl...The dihydric dithioketenes 3a-c obtained by 1,2-addition of methallyl Grignard reagent to bis(alkylthio)methylidene derivative ofdimedone 2a-c wewr converted to the cycloaromatization product 4 assisted by boron trifluoride etherate.When this reaction was performed in methanol,the substitution-cycloaroatization product 5 was obtained as by- product from 3c.To this eycloaromatization reaction,,the reactivity order dimethylthio>1, 3 - propylenedithio>1, 2- ethylenedithio carbon cation was established by the yields from 3a-c 4.An intramolecular a1,a1reaction pattern was developed by experiment.展开更多
The synthesis of heterometallic aluminum-based materials is challenging yet attractive,due to their potential applications in optics,catalysis,magnetism and semiconductor device.We have now successfully synthesized tw...The synthesis of heterometallic aluminum-based materials is challenging yet attractive,due to their potential applications in optics,catalysis,magnetism and semiconductor device.We have now successfully synthesized two Al,Niz heterometallic clusters bearing different peripheral alkoxide ligands through a heterometal substitution strategy.展开更多
This research on the solvent effects of 2 methyl 4,5 dimethoxy 3 oxo 2H pyridizine (MDOP) in binary solvent systems on the infrared spectra for MDOP in n hexane/CHCl 3 mixture solvents showed that there were ...This research on the solvent effects of 2 methyl 4,5 dimethoxy 3 oxo 2H pyridizine (MDOP) in binary solvent systems on the infrared spectra for MDOP in n hexane/CHCl 3 mixture solvents showed that there were three forms of carbonyl stretching vibration band [ υ (C=O)] of MPOP as the mole fraction of CHCl 3 in the binary solvents changes. In pure n hexane solvent, the υ (C=O) of MDOP appeared at a relatively high wavenumber. With CHCl 3 added, the υ (C=O) shifted to lower wavenumbers. Two new bands were observed over a certain range of mixture solvent compositions. The origin of the bands was discussed in the terms of two kinds of hydrogen bond together with their individual dependence on mixture composition. Comparisons were drawn for the solvent sensitivities of υ (C=O) for propanone.展开更多
The γ-oxo vinyliminophosphorane 3 was prepared for the first time from the Staudinger reaction of vinyl azide 2 and triphenylphosphine. The reaedvity of 3 was studied
Triazolylenzoylketene S.S-acetial(1) reacted with aniline to S, N-acetal (2). with ethylenediamine, o-phenylenediamine and ethanolamine to the corresponding cyclic N, N-acetals(3), (5) and N, O-acetal(1). Treatment of...Triazolylenzoylketene S.S-acetial(1) reacted with aniline to S, N-acetal (2). with ethylenediamine, o-phenylenediamine and ethanolamine to the corresponding cyclic N, N-acetals(3), (5) and N, O-acetal(1). Treatment of (1), (2) with guanidine and hydrazine led in the biheteroeycles(6). (7). (8)respectively展开更多
文摘Nine indole alkaloids and one aromatic amine were isolated from Evodia rutaecarpa Benth. Their structures were identified as evodiamine(1),rutaecarpine(2),formyldihydrorutaecarpine(3),goshuyuamide I(4),evodiamide(5),hydroxyevodiamine(6),β carboline(7),1,2,3,4 tetrahydro 1 oxo β carboline(8),dehydroevodiamine(9)and N methylanthranylamide(10).Compound 8 was a new natural product. Compound 7 was for the first time isolated from Evodia.
文摘The title compound (C_ 24H_ 40Cl_6O_ 16V_3, M_r = 950.08) was synthesized from the reaction of VCl_3 and NaO_2CEt in CHCl_3 and THF. The crystal structure has been determined by X-ray single-crystal diffraction analysis. It crystallizes in monoclinic space group C2/c with a = 12.5768(4), b= 16.5601(4), c = 19.3574(7) , β = 99.879(1)°, V = 3971.3(2)3, D_c = 1.589 g/cm3, μ= 1.157 mm -1, F(000)=1932, Z=4, R = 0.055, wR = 0.1539 (I2σ(I)). This compound has an unusual coplanar V_3O core with a C_2 axis passing through O(1), V(1), O(10): one V-μ_3O is short (1.628 ), the other two are longer (2.381 ). It was characterized by IR, 1H NMR, and EPR spectra. It was unstable and the decomposition process of this compound was studied using IR spectroscopy.
基金Supported by the foundation of Education Committee of Fujian Province (JB01045)
文摘The title compound [Ni(bipy)3][(-oxo)Fe2Cl6] (bipy = 2, 2?bispyridine) was synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group P2l/c with unit cell parameters: a = 9.7085(7),b = 26.409(2), c = 14.014(1) ,?= 100.237(3), V = 3535.9(2) 3,Z = 4,C30H24Cl6Fe2N6NiO,Mr = 867.66, Dc = 1.630 g/cm3,F(000) = 1744, (MoK? = 1.824 mm-1, the final R = 0.0394 and wR = 0.0475 for 2750 observed reflections with I ≥ 2(I). The title compound contains cation of [Ni(bipy)3]2+ and anion of [(-oxo)Fe2Cl6] 2- which consists of two [FeCl3] fragments connected by an oxo bridge with the bond distances of Fe(2)O(1) 1.752(2) and Fe(1)O(1) 1.763(2) , and the bond angle of Fe(2)O(1)Fe(1) 148.6(2)? In the [Fe2(-oxo)Cl6]2- complex, the two iron(Ⅲ) centers exhibit a tetrahedral coordination with the distorted tetrahedron formed by three Cl atoms and one oxo bridge.
文摘The single crystals of the title quaternary compound were synthesized by solid state reaction at 950℃ from SmOBr-V-NH_4Cl system.It crystallized in monoclinic system,space group C2/M with cell dimmensions of a=1.3255(2) nm.b=0. 5588(5) nm, c=1.0942(5) nm;β=100.48(2)°;Γ=0.797(1) nm3; Z=2; Dc= 5.50 g/cm3 ; F(000) = 1190; μ(MoKα)=176.82cm-1.The final R and Rw for 1430 reflections with I>3.00 σ(I) were 0.071 and0.085 respectively.The Sm atoms are 8-coordinated.the V atoms have octahedral coordination environment and the Si atoms are tetrahedral.The structure of the title compound is built from vanadium octahedra layers and samarium-vanadium-silicate slabs.
文摘A novel polyester containing glycolic acid(GA)and 2 hydro 2 oxo 1,3,2 dioxaphosphorinane(TMP)was prepared by ring opening polymerization.The composition and the structure of the titled polymer were investigated by 1H NMR, 13 C NMR,FT IR,EA,and VPO.The influence of time on total conversion and molecular weight was also studied.
文摘The reaction mechanism of OXO(X=Cl, Br) with H(2\%S\%) was studied theoretically by using the B3LYP/6-311+G(3df, 3pd) and the high-level electron-correlation QCISD(T)/6-311+G ** at single-point. The results show that the mechanism for the title reaction involves three channels, from which OH+XO, HO 2+X and HX+O 2 products could be obtained, respectively. Therefore, the channel to yield the products OH+XO is the dominant one in agreement with the experiments.
基金supported by the Knowledge Innovation Program of the Chinese Academy of Sciences (Grant: DICP K2000B3)
文摘Mesoporous zirconium oxo phosphate-sulfate was synthesized by hydrothermal method with hexadecyltrithylammonium bromide(CTAB)as the template and with zirconium nitrate or zirconium oxychloride as zirconium source.The optimum two-stage process was established, ^(31)P MAS NMR showed that the states of phosphate species were changed with further postsynthesis treatment by sulfate acid. The transformations of the structures at different temperatures from room temperature to 1173 K were investigated by XRD. ...
文摘o-Carboxybenzaldehyde (1)and acetone gave the Claisen-Schmidt condensation product, which readily cyclizes on acidification to give 1-oxo-3-acetonyl-dihydrobenzo [c]furan(4)in 68% yield. Other methyl ketones behaved similarly.
基金Supported by the Ministerio De Ciencia Y Technologia(NoSB2004-oobo)
文摘A variety of gold（Ⅲ） adducts having a-ligated oxygen-donor ligands have been prepared from [Au（ppy）Cl2]（ppy.phenylpyridine）（1） either by partial or total replacement of the chloride ions. The new species comprise hydroxo-[Au（ppy）（OH）Cl]（2）, and [Au（ppy）（OH）2]（3）, oxo-[Au2（ppy）2（μ-O）2]（4）, acetate-[Au（ppy）（O2CMe2）] （5）, and alkoxo complexes-[Au（ppy）（OR）Cl]（6, 7） and [Au（ppy）（OR）2]（8--10）（R=Me, 6 and 8; Et, 7 and 9; Pr, 10）. The dihydroxo and the oxo complexes can be interconverted by refluxing the former in anhydrous THF and the latter in water. The hydroxides 2 and 3 and the acetato complex 5 undergo σ-ligand metathesis in ROH solution（R=Me, Et or Pr） to give the corresponding alkoxides.
文摘The dihydric dithioketenes 3a-c obtained by 1,2-addition of methallyl Grignard reagent to bis(alkylthio)methylidene derivative ofdimedone 2a-c wewr converted to the cycloaromatization product 4 assisted by boron trifluoride etherate.When this reaction was performed in methanol,the substitution-cycloaroatization product 5 was obtained as by- product from 3c.To this eycloaromatization reaction,,the reactivity order dimethylthio>1, 3 - propylenedithio>1, 2- ethylenedithio carbon cation was established by the yields from 3a-c 4.An intramolecular a1,a1reaction pattern was developed by experiment.
基金This work is supported by the National Natural Science Foundation of China(92061104,21935010 and 21973096)the Natural Science Foundation of Fujian Province(2021J06035)the Youth Innovation Promotion Association CAS(Y2018081).
文摘The synthesis of heterometallic aluminum-based materials is challenging yet attractive,due to their potential applications in optics,catalysis,magnetism and semiconductor device.We have now successfully synthesized two Al,Niz heterometallic clusters bearing different peripheral alkoxide ligands through a heterometal substitution strategy.
文摘This research on the solvent effects of 2 methyl 4,5 dimethoxy 3 oxo 2H pyridizine (MDOP) in binary solvent systems on the infrared spectra for MDOP in n hexane/CHCl 3 mixture solvents showed that there were three forms of carbonyl stretching vibration band [ υ (C=O)] of MPOP as the mole fraction of CHCl 3 in the binary solvents changes. In pure n hexane solvent, the υ (C=O) of MDOP appeared at a relatively high wavenumber. With CHCl 3 added, the υ (C=O) shifted to lower wavenumbers. Two new bands were observed over a certain range of mixture solvent compositions. The origin of the bands was discussed in the terms of two kinds of hydrogen bond together with their individual dependence on mixture composition. Comparisons were drawn for the solvent sensitivities of υ (C=O) for propanone.
文摘The γ-oxo vinyliminophosphorane 3 was prepared for the first time from the Staudinger reaction of vinyl azide 2 and triphenylphosphine. The reaedvity of 3 was studied
文摘Triazolylenzoylketene S.S-acetial(1) reacted with aniline to S, N-acetal (2). with ethylenediamine, o-phenylenediamine and ethanolamine to the corresponding cyclic N, N-acetals(3), (5) and N, O-acetal(1). Treatment of (1), (2) with guanidine and hydrazine led in the biheteroeycles(6). (7). (8)respectively
