A novel Zn(Ⅱ) complex, [ZnL2(H2O)4]·H2O(1, HL = 2-(nicotinoyloxy)acetic acid), was synthesized using Zn(OAc)2·2H2O and 2-(nicotinoyloxy)acetic acid as raw materials. Its structure has been eluci...A novel Zn(Ⅱ) complex, [ZnL2(H2O)4]·H2O(1, HL = 2-(nicotinoyloxy)acetic acid), was synthesized using Zn(OAc)2·2H2O and 2-(nicotinoyloxy)acetic acid as raw materials. Its structure has been elucidated by elemental analysis, IR and single-crystal X-ray diffraction. The structural analysis revealed that complex 1 crystallizes in triclinic, space group P1 and the Zn(Ⅱ) atom is six-coordinated with two N atoms from two different 2-(nicotinoyloxy)acetate anion ligands and four O atoms from coordinated water molecules. Complex 1 forms a 3D network structure by O–H···O hydrogen bonds. The antitumor activities of 2-(nicotinoyloxy)acetic acid ligand and its Zn(Ⅱ) complex were evaluated against human lung adenocarcinoma A549 cells, human hepatoma SMMC-7721 cells and human colon carcinoma Wi Dr cells.展开更多
A new binuclear Zn^Ⅱ coordination complex,Zn2(bta)(phen)2(Cl)3(1,Hbta = 2-(1Hbenzotriazol-1-yl)acetic acid and phen = 1,10-phenanthroline),has been synthesized and characterized by single-crystal X-ray diff...A new binuclear Zn^Ⅱ coordination complex,Zn2(bta)(phen)2(Cl)3(1,Hbta = 2-(1Hbenzotriazol-1-yl)acetic acid and phen = 1,10-phenanthroline),has been synthesized and characterized by single-crystal X-ray diffraction,IR spectroscopy,elemental,and photoluminescent analysis.Complex 1 crystallizes in triclinic system,space group P1 with a = 9.3040(19),b = 10.694(2),c =16.841(3) A°,α = 101.18(3),β = 105.77(3),γ = 91.72(3)°,V= 1575.8(5) A°3,C(32)H(22)Zn2Cl3N7O2,Mr =773.66,Dc = 1.631 g/cm^3,Z = 2,F(000) = 780,μ = 1.820 mm^-1,the final R = 0.1238 and wR =0.1131.X-ray diffraction analyses indicate that 1 displays two crystallographic independent Zn^Ⅱmetal centers with a distorted tetragonal pyramidal(ZnN4O) and a tetrahedral(ZnNCl3) geometries,respectively.The phen serves as a common N,N'-bidentate ligand,and the bta^- as a unique N,O-bridged ligand in 1.In the crystal,1 forms a stable 3D supramolecular architecture by trifurcated hydrogen bonding C-H…C1 interactions and C-H…π,π…π stacking.1 showed photo-electric conversion properties.展开更多
A new series of compounds, 2-(benzodioxol-2-yl)acetic acids, have been synthesized. Their structures were confirmed by MS and 1H-NMR. The preliminary pharmacological screening showed that these compounds exhibited p...A new series of compounds, 2-(benzodioxol-2-yl)acetic acids, have been synthesized. Their structures were confirmed by MS and 1H-NMR. The preliminary pharmacological screening showed that these compounds exhibited potent human PPARδ agonist activities.展开更多
A new compound 2-(3,5-di-tert-butyl-2-hydroxyphenyl)-2-(3,4-dimethylphenyl) acetic acid dimethylamine salt ([NH2(CH3)2][C24H31O3]) was synthesized and structurally determined. It is of monoclinic system, space...A new compound 2-(3,5-di-tert-butyl-2-hydroxyphenyl)-2-(3,4-dimethylphenyl) acetic acid dimethylamine salt ([NH2(CH3)2][C24H31O3]) was synthesized and structurally determined. It is of monoclinic system, space group P21/c with a = 14.731(2), b = 10.1185(10), c = 17.065(2) A^°, β = 98.293(10)° ,Z = 4, V = 2517.0(6)A^°^3, Dc = 1.091 g/cm^3, F(000) = 904 and Mr= 413.58. The dihedral angle defined by two benzene rings is 98.23°.展开更多
The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-(4-quinoxalin- 2-yl-phenoxy)-tetrahydro-pyran-4-yl-ester 8 (C28H28N2O10, Mr = 552.54), has been synthesized and its crystal structure was determined ...The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-(4-quinoxalin- 2-yl-phenoxy)-tetrahydro-pyran-4-yl-ester 8 (C28H28N2O10, Mr = 552.54), has been synthesized and its crystal structure was determined by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21, a = 10.060(8), b = 5.648(4), c = 24.11(2)A, β = 91.078(10)°, Z = 2, V= 1369.9(19)A^3, Dc = 1.339 g/cm^3,μ(MoKa) = 1.03 cm^-1, F(000) = 580.00, T =. 193.1 Kx-9 θmax = 25.03, (△/σ)max = 0.0000, Flack = -0.0(24), the final R = 0.0680 and wR = 0.140 (w = 1/[0.0016Fo^2 + 1.00000(Fo^2)]/(4Fo^2)) for 3126 observed reflections (1 〉 20(/)). The pyranoid ring adopts chair conformation in the sugar moiety, and all of the acetyl groups are in the e bond of the pyranoid ring, so the sugar moiety is very stable.展开更多
A novel copper(Ⅱ) complex with tert-butyl 2-[N-(tert-butyloxycarbonylmethyl)-2-picolyamino]acetate(ampy) was synthesized and structurally characterized by elemental analysis, FT-IR spectrum, electrospray ioniza...A novel copper(Ⅱ) complex with tert-butyl 2-[N-(tert-butyloxycarbonylmethyl)-2-picolyamino]acetate(ampy) was synthesized and structurally characterized by elemental analysis, FT-IR spectrum, electrospray ionization-mass spectrometry, UV-vis spectrum and single-crystal X-ray diffraction, respectively. A mononuclear copper(II) complex with ampy, [Cu(ampy)Cl2](1), was formed irrespective of the metal-to-ligand molar ratios([Cu2+]:[ampy] = 0.5:1, 1:1, and 2:1) as a single product. Complex 1 crystallizes in the orthorhombic system, space group Pbca with a = 12.343(2), b = 18.928(3), c = 20.058(4) A, V = 4686.1(14) A3, Z = 8, Dc = 1.3349(4) g/cm3, F(000) = 1920, S = 1.016, R = 0.0693 and w R = 0.1721 for 3151 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that the central copper(II) ion is bound by pyridyl N, tertiary amine N and carbonyl O atoms of the quadridentate ampy as well as two Cl anions, constructing a slightly distorted octahedral geometry. Complex 1 further constructs a stable 3D supramolecular architecture by intermolecular C–H…Cl hydrogen bonds. In addition, the molecular geometry was calculated by density functional theory(DFT/B3LYP) method with the basis sets(6-31+G(d,p) for H, C, N, O and Cl atoms, and LANL2 DZ for Cu atom, respectively). The calculated results show that the optimized geometrical parameters are in good agreement with the experimental data. Natural bond orbital(NBO) analysis and frontier molecular orbitals(FMOs) analysis were investigated at the same level.展开更多
The title compound was synthesized by the base catalyzed reaction of 5-((quinolin- 8-yloxy)methyl)-1,3,4-oxadiazole-2(3H)-thione with methyl chloroacetate. The structure was supported by the spectroscopic data a...The title compound was synthesized by the base catalyzed reaction of 5-((quinolin- 8-yloxy)methyl)-1,3,4-oxadiazole-2(3H)-thione with methyl chloroacetate. The structure was supported by the spectroscopic data and unambiguously confirmed by single-crystal X-ray diffraction studies. It crystallizes from a methanol solution in the triclinic space group Pi with unit cell dimensions a = 7.4509(9), b = 10.2389(12), c = 12.2299(15)A, a = 74.771(2), β = 77.956(2), 7 = 69.263(2)°, V = 834.98(17) A3 and Z = 2. In order to gain some valuable insights into the molecular structure, the quantum mechanical calculations were performed using both HF and time-dependent density functional theory at the B3LYP/6-31G(d,p) level. The molecular geometry from X-ray determination of the title compound in the ground state has been compared using the Hartree-Fock (HF) and density functional theory (DFT) with the 6-31G(d) basis set. The calculated results show that the DFT and HF can well reproduce the structure of the title compound. The energetic behavior of the title compound was examined using the B3LYP method with the 6-31G(d) basis set. The harmonic vibrational frequencies calculated have been compared with the experimental FTIR and FT-Raman spectra. The restricted Hartree-Fock and density functional theory-based nuclear magnetic resonance (NMR) calculation procedure was also performed, and it was used for assigning the 13C and 1H NMR chemical shifts of the title compound. Moreover, molecular electrostatic potential and thermodynamic parameters of the title compound were investigated by theoretical calculations.展开更多
The new title compound, chiral 2-(3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl)- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been conf...The new title compound, chiral 2-(3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl)- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been confirmed by IR, 1H NMR, 13C NMR, LC-MS (ESI) and single-crystal X-ray diffraction. (R)-2-(3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl)-2-oxoethyl acetate crystallizes in monoclinic, space group P21/c with a = 11.867(2), b = 8.4087(2), c = 14.325(6) A^°, β = 117.59(2)°, Z = 4, V = 1266.9(6) A^°3, Dc = 1.307 g/cm^3, F(000) = 528, μ(MoKα) = 0.097 mm-1, R = 0.0453 and wR = 0.1237; (S)-2-(3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl)-2-oxoethyl acetate belongs to the triclinic system, space group P with a = 8.2647(17), b = 8.7034(17), c = 9.5479(19) A^°, α = 105.33(3), β = 100.95(3), γ = 105.14(3)°, Z = 2, V = 614.1(2) A^°3, Dc = 1.348 g/cm^3, F(000) = 264, μ(MoKα) = 0.10 mm-1, R = 0.0613 and wR = 0.1037. Both of the molecules prefer to form crystal packing through C–H…O hydrogen bonds.展开更多
We substituted several environmentally friendly catalysts which included HY and H- β zeolites, various cation-exchanged β zeolites, and solid-supported ferric chloride for conventional catalysts for the synth...We substituted several environmentally friendly catalysts which included HY and H- β zeolites, various cation-exchanged β zeolites, and solid-supported ferric chloride for conventional catalysts for the synthesis of 3-(1-cyclohexenyl)-2-butanone from the reaction of ethylidenecyclohexane with acetic anhydride at room temperature. HY zeolite was found to be the most effective for this reaction, and gave the acylated product in a 72% yield under the conditions of n (ethylidenecyclohexane)/ n (acetic anhydride)/ m (HY zeolite)=1 mmol/10 mmol/0 100 g, reaction temperature 25 ℃ and reaction time 2 h. The used HY zeolite can be recovered, regenerated and gave almost the same yield as the fresh one. The lifetime of the HY zeolite is over 80 h. The effect of different factors on the reaction has also been investigated.展开更多
To investigate the relationship between the expression of cyclooxygenase-2 (COX-2) and menstrual cycle, the regulatory effects of 17-β-estradiol (E2) and medroxyprogesterone acetate (MPA) on the expression of C...To investigate the relationship between the expression of cyclooxygenase-2 (COX-2) and menstrual cycle, the regulatory effects of 17-β-estradiol (E2) and medroxyprogesterone acetate (MPA) on the expression of COX-2 in cervical cancer Hela cells were examined. Cervical cancer specimens were obtained from 47 pre-menopausal patients. The phase of menstrual cycle was determined by case history and HE staining of uterine endometrium. COX-2 was immunohistochemically stained by SABC staining and the staining intensity was determined with computerized image analysis system. Hela cells were incubated with alcohol, E2, E2+MPA, MPA for 12, 24 and 48 h respectively. The expression of COX-2 in Hela cells was detected by Western blotting and reverse transcriptase-polymerase chain reaction (RT-PCR). Our results showed that the expression of COX-2 was significantly higher during proliferative phase than secretory phase (P〈0.05), but there was no difference in the positive rate between proliferative phase and secretory phase (P〉0.05). Incubation with E2 could significantly enhance the expression of COX-2 continually. On the contrary, E2+MPA and MPA alone could decrease the expression of COX-2 as compared with the control and E2 group (P〈0.05 and P〈0.01 respectively). It is concluded that the expression of COX-2 in cervical cancer of pre-menopausal patients and Hela cells was regulated by estrogen/progestogen.展开更多
In order to quantitate dencichine in biological samples, a selective and sensitive method for the determination of dencichine in rat plasma based on high-performance liquid chromatography-tandem mass spectrometry (HPL...In order to quantitate dencichine in biological samples, a selective and sensitive method for the determination of dencichine in rat plasma based on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed and validated. (l)-2-amino-3-(carboxymethylthio)propionic acid was used as the internal standard (I.S.). After a protein precipitation extraction with acetonitrile, dencichine and the I.S. were chromatographed on an Xterra MS-C18 column. The mobile phase was consisted of 20mmol/L ammonium acetate solution-acetonitrile (35:65, V/V) at a flow rate of 0.2 mL/min. The detection was performed on a triple quadrupole mass via electrospray ionization (ESI) source in the positive mode. The intra- and inter-day precision (relative standard deviation, R.S.D.) values of dencichine were below 6.7%. The extraction recoveries were up 85%. The lower limit of quantification was 20 ng/ml, which was sensitive enough to detect the analyte. The HPLC-MS/MS method was successfully applied to the pharmacokinetic study after an intravenous administration of dencichine in Sprague-Dawley (SD) rat.展开更多
A new energetic material, 4,5-diacetoxyl-2-(dinitromethylene)-imidazolidine (DADNI), was synthesized by the reaction of 4,5-dihydroxyl-2-(dinitromethylene)-imidazolidine (DDNI) and acetic anhydride, and charac...A new energetic material, 4,5-diacetoxyl-2-(dinitromethylene)-imidazolidine (DADNI), was synthesized by the reaction of 4,5-dihydroxyl-2-(dinitromethylene)-imidazolidine (DDNI) and acetic anhydride, and characterized by single crystal X-ray diffraction. Crystal data for DADNI are monoclinic, space group C2/c, a= 15.9167(3)A, b= 8.6816(4)A, c=8.5209(3) A, t= 103.294(9)°, V= 1145.9(3) A3, Z=4,A=0.150 mm 1, F(000)=600, Dc= 1.682 gocm-3, R] =0.0565 and wR2=0.1649. Thermal decomposition behavior of DADNI was studied and an intensely exothermic process was observed. The kinetic equation of the decomposition reaction is:exp(-1.582 ×10^5/RT). The critical temperature of thermal explosion is 163.76℃. The specific heat capacity of DADNI was studied with micro-DSC method and theoretical calculation method. The molar heat capacity is 343.30 J·mol^-1·K^-1 at 298.15 K. The adiabatic time-to-explosion of DADNI was calculated to be 87.7 s.展开更多
基金supported by the National Natural Science Foundation of China(No.21171132)the Project of Shandong Province Higher Educational Science and Technology Program(J14LC01)Science Foundation of Weifang
文摘A novel Zn(Ⅱ) complex, [ZnL2(H2O)4]·H2O(1, HL = 2-(nicotinoyloxy)acetic acid), was synthesized using Zn(OAc)2·2H2O and 2-(nicotinoyloxy)acetic acid as raw materials. Its structure has been elucidated by elemental analysis, IR and single-crystal X-ray diffraction. The structural analysis revealed that complex 1 crystallizes in triclinic, space group P1 and the Zn(Ⅱ) atom is six-coordinated with two N atoms from two different 2-(nicotinoyloxy)acetate anion ligands and four O atoms from coordinated water molecules. Complex 1 forms a 3D network structure by O–H···O hydrogen bonds. The antitumor activities of 2-(nicotinoyloxy)acetic acid ligand and its Zn(Ⅱ) complex were evaluated against human lung adenocarcinoma A549 cells, human hepatoma SMMC-7721 cells and human colon carcinoma Wi Dr cells.
基金supported by Guangxi Provincial Department of Education(No.KY2015ZD130)the Natural Science Foundation of Guangxi Province(No.2013GXNSFBA019030)the financial support from the Natural Science Foundation of Qinzhou University(No.2014PY-GJ05)
文摘A new binuclear Zn^Ⅱ coordination complex,Zn2(bta)(phen)2(Cl)3(1,Hbta = 2-(1Hbenzotriazol-1-yl)acetic acid and phen = 1,10-phenanthroline),has been synthesized and characterized by single-crystal X-ray diffraction,IR spectroscopy,elemental,and photoluminescent analysis.Complex 1 crystallizes in triclinic system,space group P1 with a = 9.3040(19),b = 10.694(2),c =16.841(3) A°,α = 101.18(3),β = 105.77(3),γ = 91.72(3)°,V= 1575.8(5) A°3,C(32)H(22)Zn2Cl3N7O2,Mr =773.66,Dc = 1.631 g/cm^3,Z = 2,F(000) = 780,μ = 1.820 mm^-1,the final R = 0.1238 and wR =0.1131.X-ray diffraction analyses indicate that 1 displays two crystallographic independent Zn^Ⅱmetal centers with a distorted tetragonal pyramidal(ZnN4O) and a tetrahedral(ZnNCl3) geometries,respectively.The phen serves as a common N,N'-bidentate ligand,and the bta^- as a unique N,O-bridged ligand in 1.In the crystal,1 forms a stable 3D supramolecular architecture by trifurcated hydrogen bonding C-H…C1 interactions and C-H…π,π…π stacking.1 showed photo-electric conversion properties.
基金supported by the National High Technology Research and Development Program of China(863 project:2003AA235010)the National Natural Science Foundation of China(No.30472092).
文摘A new series of compounds, 2-(benzodioxol-2-yl)acetic acids, have been synthesized. Their structures were confirmed by MS and 1H-NMR. The preliminary pharmacological screening showed that these compounds exhibited potent human PPARδ agonist activities.
基金supported by the Technology Risk Innovation Fund of PetroChina Company Ltd.
文摘A new compound 2-(3,5-di-tert-butyl-2-hydroxyphenyl)-2-(3,4-dimethylphenyl) acetic acid dimethylamine salt ([NH2(CH3)2][C24H31O3]) was synthesized and structurally determined. It is of monoclinic system, space group P21/c with a = 14.731(2), b = 10.1185(10), c = 17.065(2) A^°, β = 98.293(10)° ,Z = 4, V = 2517.0(6)A^°^3, Dc = 1.091 g/cm^3, F(000) = 904 and Mr= 413.58. The dihedral angle defined by two benzene rings is 98.23°.
基金This project was supported by the Key Laboratory of Organic Synthesis of Jiangsu Province
文摘The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-(4-quinoxalin- 2-yl-phenoxy)-tetrahydro-pyran-4-yl-ester 8 (C28H28N2O10, Mr = 552.54), has been synthesized and its crystal structure was determined by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21, a = 10.060(8), b = 5.648(4), c = 24.11(2)A, β = 91.078(10)°, Z = 2, V= 1369.9(19)A^3, Dc = 1.339 g/cm^3,μ(MoKa) = 1.03 cm^-1, F(000) = 580.00, T =. 193.1 Kx-9 θmax = 25.03, (△/σ)max = 0.0000, Flack = -0.0(24), the final R = 0.0680 and wR = 0.140 (w = 1/[0.0016Fo^2 + 1.00000(Fo^2)]/(4Fo^2)) for 3126 observed reflections (1 〉 20(/)). The pyranoid ring adopts chair conformation in the sugar moiety, and all of the acetyl groups are in the e bond of the pyranoid ring, so the sugar moiety is very stable.
基金supported by the National Basic Research Program of China(No.2014CB643401)the National Natural Science Foundation of China(Nos.51134007 and 51474256)
文摘A novel copper(Ⅱ) complex with tert-butyl 2-[N-(tert-butyloxycarbonylmethyl)-2-picolyamino]acetate(ampy) was synthesized and structurally characterized by elemental analysis, FT-IR spectrum, electrospray ionization-mass spectrometry, UV-vis spectrum and single-crystal X-ray diffraction, respectively. A mononuclear copper(II) complex with ampy, [Cu(ampy)Cl2](1), was formed irrespective of the metal-to-ligand molar ratios([Cu2+]:[ampy] = 0.5:1, 1:1, and 2:1) as a single product. Complex 1 crystallizes in the orthorhombic system, space group Pbca with a = 12.343(2), b = 18.928(3), c = 20.058(4) A, V = 4686.1(14) A3, Z = 8, Dc = 1.3349(4) g/cm3, F(000) = 1920, S = 1.016, R = 0.0693 and w R = 0.1721 for 3151 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that the central copper(II) ion is bound by pyridyl N, tertiary amine N and carbonyl O atoms of the quadridentate ampy as well as two Cl anions, constructing a slightly distorted octahedral geometry. Complex 1 further constructs a stable 3D supramolecular architecture by intermolecular C–H…Cl hydrogen bonds. In addition, the molecular geometry was calculated by density functional theory(DFT/B3LYP) method with the basis sets(6-31+G(d,p) for H, C, N, O and Cl atoms, and LANL2 DZ for Cu atom, respectively). The calculated results show that the optimized geometrical parameters are in good agreement with the experimental data. Natural bond orbital(NBO) analysis and frontier molecular orbitals(FMOs) analysis were investigated at the same level.
文摘The title compound was synthesized by the base catalyzed reaction of 5-((quinolin- 8-yloxy)methyl)-1,3,4-oxadiazole-2(3H)-thione with methyl chloroacetate. The structure was supported by the spectroscopic data and unambiguously confirmed by single-crystal X-ray diffraction studies. It crystallizes from a methanol solution in the triclinic space group Pi with unit cell dimensions a = 7.4509(9), b = 10.2389(12), c = 12.2299(15)A, a = 74.771(2), β = 77.956(2), 7 = 69.263(2)°, V = 834.98(17) A3 and Z = 2. In order to gain some valuable insights into the molecular structure, the quantum mechanical calculations were performed using both HF and time-dependent density functional theory at the B3LYP/6-31G(d,p) level. The molecular geometry from X-ray determination of the title compound in the ground state has been compared using the Hartree-Fock (HF) and density functional theory (DFT) with the 6-31G(d) basis set. The calculated results show that the DFT and HF can well reproduce the structure of the title compound. The energetic behavior of the title compound was examined using the B3LYP method with the 6-31G(d) basis set. The harmonic vibrational frequencies calculated have been compared with the experimental FTIR and FT-Raman spectra. The restricted Hartree-Fock and density functional theory-based nuclear magnetic resonance (NMR) calculation procedure was also performed, and it was used for assigning the 13C and 1H NMR chemical shifts of the title compound. Moreover, molecular electrostatic potential and thermodynamic parameters of the title compound were investigated by theoretical calculations.
基金supported by the National Natural Science Foundation of China(No.31572042)Natural Science Foundation of Heilongjiang Province(B201303)the Research Science Foundation in Technology Innovation of Harbin(No.2015RAYXJ010)
文摘The new title compound, chiral 2-(3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl)- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been confirmed by IR, 1H NMR, 13C NMR, LC-MS (ESI) and single-crystal X-ray diffraction. (R)-2-(3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl)-2-oxoethyl acetate crystallizes in monoclinic, space group P21/c with a = 11.867(2), b = 8.4087(2), c = 14.325(6) A^°, β = 117.59(2)°, Z = 4, V = 1266.9(6) A^°3, Dc = 1.307 g/cm^3, F(000) = 528, μ(MoKα) = 0.097 mm-1, R = 0.0453 and wR = 0.1237; (S)-2-(3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl)-2-oxoethyl acetate belongs to the triclinic system, space group P with a = 8.2647(17), b = 8.7034(17), c = 9.5479(19) A^°, α = 105.33(3), β = 100.95(3), γ = 105.14(3)°, Z = 2, V = 614.1(2) A^°3, Dc = 1.348 g/cm^3, F(000) = 264, μ(MoKα) = 0.10 mm-1, R = 0.0613 and wR = 0.1037. Both of the molecules prefer to form crystal packing through C–H…O hydrogen bonds.
基金Supported by the National Natural Science Foundation of China( No.2 0 1730 14 )
文摘We substituted several environmentally friendly catalysts which included HY and H- β zeolites, various cation-exchanged β zeolites, and solid-supported ferric chloride for conventional catalysts for the synthesis of 3-(1-cyclohexenyl)-2-butanone from the reaction of ethylidenecyclohexane with acetic anhydride at room temperature. HY zeolite was found to be the most effective for this reaction, and gave the acylated product in a 72% yield under the conditions of n (ethylidenecyclohexane)/ n (acetic anhydride)/ m (HY zeolite)=1 mmol/10 mmol/0 100 g, reaction temperature 25 ℃ and reaction time 2 h. The used HY zeolite can be recovered, regenerated and gave almost the same yield as the fresh one. The lifetime of the HY zeolite is over 80 h. The effect of different factors on the reaction has also been investigated.
文摘To investigate the relationship between the expression of cyclooxygenase-2 (COX-2) and menstrual cycle, the regulatory effects of 17-β-estradiol (E2) and medroxyprogesterone acetate (MPA) on the expression of COX-2 in cervical cancer Hela cells were examined. Cervical cancer specimens were obtained from 47 pre-menopausal patients. The phase of menstrual cycle was determined by case history and HE staining of uterine endometrium. COX-2 was immunohistochemically stained by SABC staining and the staining intensity was determined with computerized image analysis system. Hela cells were incubated with alcohol, E2, E2+MPA, MPA for 12, 24 and 48 h respectively. The expression of COX-2 in Hela cells was detected by Western blotting and reverse transcriptase-polymerase chain reaction (RT-PCR). Our results showed that the expression of COX-2 was significantly higher during proliferative phase than secretory phase (P〈0.05), but there was no difference in the positive rate between proliferative phase and secretory phase (P〉0.05). Incubation with E2 could significantly enhance the expression of COX-2 continually. On the contrary, E2+MPA and MPA alone could decrease the expression of COX-2 as compared with the control and E2 group (P〈0.05 and P〈0.01 respectively). It is concluded that the expression of COX-2 in cervical cancer of pre-menopausal patients and Hela cells was regulated by estrogen/progestogen.
文摘In order to quantitate dencichine in biological samples, a selective and sensitive method for the determination of dencichine in rat plasma based on high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed and validated. (l)-2-amino-3-(carboxymethylthio)propionic acid was used as the internal standard (I.S.). After a protein precipitation extraction with acetonitrile, dencichine and the I.S. were chromatographed on an Xterra MS-C18 column. The mobile phase was consisted of 20mmol/L ammonium acetate solution-acetonitrile (35:65, V/V) at a flow rate of 0.2 mL/min. The detection was performed on a triple quadrupole mass via electrospray ionization (ESI) source in the positive mode. The intra- and inter-day precision (relative standard deviation, R.S.D.) values of dencichine were below 6.7%. The extraction recoveries were up 85%. The lower limit of quantification was 20 ng/ml, which was sensitive enough to detect the analyte. The HPLC-MS/MS method was successfully applied to the pharmacokinetic study after an intravenous administration of dencichine in Sprague-Dawley (SD) rat.
基金Project supported by the National Natural Science Foundation of China (No. 20803058), Basal Science Foundation of National Defense (No. B0920110005) and the Education Committee Foundation of Shaanxi Province (No. 2010JK881).
文摘A new energetic material, 4,5-diacetoxyl-2-(dinitromethylene)-imidazolidine (DADNI), was synthesized by the reaction of 4,5-dihydroxyl-2-(dinitromethylene)-imidazolidine (DDNI) and acetic anhydride, and characterized by single crystal X-ray diffraction. Crystal data for DADNI are monoclinic, space group C2/c, a= 15.9167(3)A, b= 8.6816(4)A, c=8.5209(3) A, t= 103.294(9)°, V= 1145.9(3) A3, Z=4,A=0.150 mm 1, F(000)=600, Dc= 1.682 gocm-3, R] =0.0565 and wR2=0.1649. Thermal decomposition behavior of DADNI was studied and an intensely exothermic process was observed. The kinetic equation of the decomposition reaction is:exp(-1.582 ×10^5/RT). The critical temperature of thermal explosion is 163.76℃. The specific heat capacity of DADNI was studied with micro-DSC method and theoretical calculation method. The molar heat capacity is 343.30 J·mol^-1·K^-1 at 298.15 K. The adiabatic time-to-explosion of DADNI was calculated to be 87.7 s.