Palladium-catalyzed the Sonogashira coupling reaction of 3-halogen-2-aminopyridines 1 with terminal alkynes 2 afforded the corresponding 21 target products 3a-3u in the presence of palladium catalyst. The structure of...Palladium-catalyzed the Sonogashira coupling reaction of 3-halogen-2-aminopyridines 1 with terminal alkynes 2 afforded the corresponding 21 target products 3a-3u in the presence of palladium catalyst. The structure of target products 3a-3u was confirmed and characterized by 1H NMR, 13C NMR, and HRMS. The influences of different kinds of catalyst loading, bases, substrates and temperature were also investigated. Under the optimized conditions, including 2.5 mol% Pd?(CF3COO)2, 5 mol% PPh3 and 5 mol% CuI as additive, 1 mL Et3N, substrate 1 with terminal alkynes 2 for the cross-coupling reactions at 100°C for 3 h in DMF afforded the corresponding products of 2-amino-3-alkynylpyridines 3 in moderate to excellent yields (72%?-?96%). The present methodology has provided an effective synthetic method including operational convenience, high efficiency and wide-application.展开更多
Objectives To investigate the possible role of amino-terminal pro-brain natriuretic peptide （NT-proBNP） in the occurrence of atrial fibrillation （AF） after coronary artery bypass grafting （CABG）. Methods This st...Objectives To investigate the possible role of amino-terminal pro-brain natriuretic peptide （NT-proBNP） in the occurrence of atrial fibrillation （AF） after coronary artery bypass grafting （CABG）. Methods This study group included 70 consecutive patients scheduled for elective off-pump CABG. The patients with ejection fraction （EF） less than 0. 30, history of AF, use of class Ⅰ or Ⅲ antiarrhythmic drug, implanted pacemaker, postoperative myocardial infarction or chest reopening for pericardial tamponade were excluded. Preoperative and postoperative serum NT-proBNP levels were measured by radioimmunoassay technique. Results Postoperative AF occurred in 15 patients （21.4%）; these patients had significantly higher median NT-proBNP levels when compared with those without AF after the operation （ P 〈 0. 01 ）. Using multivariate logistic regression analyses, an increase in NT-proBNP level after CABG was found to be independently associated with AF （ OR = 3.78, 95% IC = 1.81 - 4. 89, P 〈 0. 01 ）. Increased age, diabetes mellitus, preoperative use of β-blocker, proximal right coronary artery involvement, and longer operation time were al- so associated with AF. Conclusions These results indicated that AF was associated with higher NT-proBNP concentrations after off pump CABG; the increase in NT-proBNP after CABG may play an important role in the occurrence of AF after the operation. The further studies are needed to define the reason that lead to higher NT-proBNP concentrations among the patients who present AF after off pump CABG.展开更多
The title compound trans-4-[（5-（2,4-dichlorophenoxy）-3-methyl- 1-phenyl-1H-pyrazol-4-yl）methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 （C28H23Cl2N5O2, Mr = 532.41） has been synthesized and its...The title compound trans-4-[（5-（2,4-dichlorophenoxy）-3-methyl- 1-phenyl-1H-pyrazol-4-yl）methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 （C28H23Cl2N5O2, Mr = 532.41） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438（4）, b = 11.6065（5）, c = 14.2215（6）A, α = 112.566（1）, β = 92.324（2）, γ = 102.91（1）°, V= 1315.65（10） A^3, Z = 2, Dc = 1.344 g/cm^3,μ（MoKa） = 0.282 mm^-1, λ = 0.71073 A, F（000） = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C（ 12）-H（12）…O（1） and C（28）-H（28）...O（1）# 1 hydrogen bonds were observed in the title compound.展开更多
A series of novel N-[α-(isoflavone-7-O-)acetyl] amino acid methyl esters were prepared from the efficient and regioselective alkylation of isoflavones with chloroacetyl amino acid derivatives under mild condition.
Enantiomers of four amino alcohols were resolved by ion-pair chromatography with (+)-10-camphorsulphonic acid as chiral counter ion. Studies of the influence of the mobile phase composition, the solute structure and t...Enantiomers of four amino alcohols were resolved by ion-pair chromatography with (+)-10-camphorsulphonic acid as chiral counter ion. Studies of the influence of the mobile phase composition, the solute structure and the mobile phase flow-rate on separation are presented. Under the optimized conditions enantiomeric propanolol, norephedrine, metropolol and salbutamol were separated using dichloromethane-1-pentanol (97:3 v/v) as mobile phase on Lichrospher-100-DIOL column.展开更多
The quantitative structure-activity relationship （QSAR） of 16 pyrazole compounds was studied by ab initio method at the HF/3-21G level using Guassian03 soft. The optimized structures together with some characteristi...The quantitative structure-activity relationship （QSAR） of 16 pyrazole compounds was studied by ab initio method at the HF/3-21G level using Guassian03 soft. The optimized structures together with some characteristic and electric parameters of the title compounds were obtained; some stereo-parameters were calculated by HyperChem software. Stepwise multiple regression method was adopted to establish bi- and tri-parametric models between biological activity and some parameters. The lager △E and logP, the higher biological activity; and the biological activity would be promoted with the smaller μ, QN and QPYRA. It provided a theory direction to synthesize some compounds with high activity.展开更多
The oxidative polycondensation reaction conditions of 4-[（4-hydroxybenzylidene） amino] phenol （4-HBAP） were studied with H2O2, air oxygen and NaOCl in an aqueous alkaline medium between 50 and 90℃. The structures...The oxidative polycondensation reaction conditions of 4-[（4-hydroxybenzylidene） amino] phenol （4-HBAP） were studied with H2O2, air oxygen and NaOCl in an aqueous alkaline medium between 50 and 90℃. The structures of the obtained monomer and polymer were confirmed by FT-IR, UV-Vis, 1H- and 13C-NMR and elemental analysis. The characterization was made by TG-DTA, size exclusion chromatography （SEC） and solubility tests. At the optimum reaction conditions, the yield of poly[4-（4-hydroxybenzylidene amino） phenol] （P-4-HBAP） was found to be 48.3% （for H2O2 oxidant）, 80.5% （for air O2 oxidant） and 86.4% （for NaOCl oxidant）. According to the SEC analysis, the number-average molecular weight （Mn）, weight-average molecular weight （Mw） and polydispersity index （PDI） values of P-4-HBAP was found to be 8950, 10970 g tool^-1 and 1.225, respectively, using H202; and l l610, 15190 g tool^-1 and 1.308 respectively, using air 02 and 7900, 9610 g mol^-1 and 1.216, respectively, using NaOC1. According to TG-DTA analyses, P-4-HBAP was more stable than 4-HBAP against thermal decomposition. The weight loss of P-4-HBAP was found to be 49.27% at 1000℃. The highest occupied molecular orbital （HOMO） and the lowest unoccupied molecular orbital （LUMO） values calculated from electrochemical measurement. Electrochemical energy gaps （Eg＇） of 4-HBAP and P-4-HBAP were found to be -5.46, -5.28; -2.26, -2.67; 3.20 and 2.61 eV, respectively. According to UV-Vis measurements, optical band gap （Eg） of 4-HBAP and P-4-HBAP were found to be 3.34 and 3.01 eV, respectively. Also, antimicrobial activities of 4-HBAP and P-4-HBAP were examined against selected some bacteria. The electrical conductivity of the polymer was measured after doping with iodine.展开更多
The purpose of this study is to use the newly synthesized molecule Sodium 8-(((carboxymethyl)amino)methyl)-4',7-bishydroxy-isoflavone-3'-sulfonate(M)as a research object,the pharmacological mechanism of the mo...The purpose of this study is to use the newly synthesized molecule Sodium 8-(((carboxymethyl)amino)methyl)-4',7-bishydroxy-isoflavone-3'-sulfonate(M)as a research object,the pharmacological mechanism of the molecule was analyzed by using a series of Systematic pharmacology methods.The results show that the M molecule has a higher drug-like DL value of 0.59 and better molecular property parameters,namely Hdon=4,Hacc=10 and AlogP=0.94;A total of 11 M molecules related targets,namely F2,ESR1,AR,F10,CA2,DPP4,CCNA2,PRSS1,CDK2,GSK3B and PTPN1;A total of 140 diseases are associated with M molecule targets,and these diseases are mainly related to cancer and cardiovascular diseases;A total of 52 pathways involve the pharmacological mechanisms of M molecules,which are mainly related to cancer and other related diseases;GO-enriched analysis showed that these targets are closely related to the regulation of peptidase activity and biological processes such as blood coagulation and hemostasis.This article clearly demonstrated the pharmacological mechanism of M molecule,which provides references for exploring the pharmacological mechanism of new compounds.展开更多
文摘Palladium-catalyzed the Sonogashira coupling reaction of 3-halogen-2-aminopyridines 1 with terminal alkynes 2 afforded the corresponding 21 target products 3a-3u in the presence of palladium catalyst. The structure of target products 3a-3u was confirmed and characterized by 1H NMR, 13C NMR, and HRMS. The influences of different kinds of catalyst loading, bases, substrates and temperature were also investigated. Under the optimized conditions, including 2.5 mol% Pd?(CF3COO)2, 5 mol% PPh3 and 5 mol% CuI as additive, 1 mL Et3N, substrate 1 with terminal alkynes 2 for the cross-coupling reactions at 100°C for 3 h in DMF afforded the corresponding products of 2-amino-3-alkynylpyridines 3 in moderate to excellent yields (72%?-?96%). The present methodology has provided an effective synthetic method including operational convenience, high efficiency and wide-application.
文摘Objectives To investigate the possible role of amino-terminal pro-brain natriuretic peptide （NT-proBNP） in the occurrence of atrial fibrillation （AF） after coronary artery bypass grafting （CABG）. Methods This study group included 70 consecutive patients scheduled for elective off-pump CABG. The patients with ejection fraction （EF） less than 0. 30, history of AF, use of class Ⅰ or Ⅲ antiarrhythmic drug, implanted pacemaker, postoperative myocardial infarction or chest reopening for pericardial tamponade were excluded. Preoperative and postoperative serum NT-proBNP levels were measured by radioimmunoassay technique. Results Postoperative AF occurred in 15 patients （21.4%）; these patients had significantly higher median NT-proBNP levels when compared with those without AF after the operation （ P 〈 0. 01 ）. Using multivariate logistic regression analyses, an increase in NT-proBNP level after CABG was found to be independently associated with AF （ OR = 3.78, 95% IC = 1.81 - 4. 89, P 〈 0. 01 ）. Increased age, diabetes mellitus, preoperative use of β-blocker, proximal right coronary artery involvement, and longer operation time were al- so associated with AF. Conclusions These results indicated that AF was associated with higher NT-proBNP concentrations after off pump CABG; the increase in NT-proBNP after CABG may play an important role in the occurrence of AF after the operation. The further studies are needed to define the reason that lead to higher NT-proBNP concentrations among the patients who present AF after off pump CABG.
基金the Science Research Foundation of Henan Institute of Science and Technology (No. 06036)
文摘The title compound trans-4-[（5-（2,4-dichlorophenoxy）-3-methyl- 1-phenyl-1H-pyrazol-4-yl）methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 （C28H23Cl2N5O2, Mr = 532.41） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438（4）, b = 11.6065（5）, c = 14.2215（6）A, α = 112.566（1）, β = 92.324（2）, γ = 102.91（1）°, V= 1315.65（10） A^3, Z = 2, Dc = 1.344 g/cm^3,μ（MoKa） = 0.282 mm^-1, λ = 0.71073 A, F（000） = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C（ 12）-H（12）…O（1） and C（28）-H（28）...O（1）# 1 hydrogen bonds were observed in the title compound.
文摘A series of novel N-[α-(isoflavone-7-O-)acetyl] amino acid methyl esters were prepared from the efficient and regioselective alkylation of isoflavones with chloroacetyl amino acid derivatives under mild condition.
文摘Enantiomers of four amino alcohols were resolved by ion-pair chromatography with (+)-10-camphorsulphonic acid as chiral counter ion. Studies of the influence of the mobile phase composition, the solute structure and the mobile phase flow-rate on separation are presented. Under the optimized conditions enantiomeric propanolol, norephedrine, metropolol and salbutamol were separated using dichloromethane-1-pentanol (97:3 v/v) as mobile phase on Lichrospher-100-DIOL column.
基金talents in University (NCET-04-0649)the Natural Science Foundation of Shandong Province (Y2006B07, Z2006B01)
文摘The quantitative structure-activity relationship （QSAR） of 16 pyrazole compounds was studied by ab initio method at the HF/3-21G level using Guassian03 soft. The optimized structures together with some characteristic and electric parameters of the title compounds were obtained; some stereo-parameters were calculated by HyperChem software. Stepwise multiple regression method was adopted to establish bi- and tri-parametric models between biological activity and some parameters. The lager △E and logP, the higher biological activity; and the biological activity would be promoted with the smaller μ, QN and QPYRA. It provided a theory direction to synthesize some compounds with high activity.
基金This work was financially supported by the TUBITAK Grants Commission for a research grant(No.TBAG-2451(104T062)).
文摘The oxidative polycondensation reaction conditions of 4-[（4-hydroxybenzylidene） amino] phenol （4-HBAP） were studied with H2O2, air oxygen and NaOCl in an aqueous alkaline medium between 50 and 90℃. The structures of the obtained monomer and polymer were confirmed by FT-IR, UV-Vis, 1H- and 13C-NMR and elemental analysis. The characterization was made by TG-DTA, size exclusion chromatography （SEC） and solubility tests. At the optimum reaction conditions, the yield of poly[4-（4-hydroxybenzylidene amino） phenol] （P-4-HBAP） was found to be 48.3% （for H2O2 oxidant）, 80.5% （for air O2 oxidant） and 86.4% （for NaOCl oxidant）. According to the SEC analysis, the number-average molecular weight （Mn）, weight-average molecular weight （Mw） and polydispersity index （PDI） values of P-4-HBAP was found to be 8950, 10970 g tool^-1 and 1.225, respectively, using H202; and l l610, 15190 g tool^-1 and 1.308 respectively, using air 02 and 7900, 9610 g mol^-1 and 1.216, respectively, using NaOC1. According to TG-DTA analyses, P-4-HBAP was more stable than 4-HBAP against thermal decomposition. The weight loss of P-4-HBAP was found to be 49.27% at 1000℃. The highest occupied molecular orbital （HOMO） and the lowest unoccupied molecular orbital （LUMO） values calculated from electrochemical measurement. Electrochemical energy gaps （Eg＇） of 4-HBAP and P-4-HBAP were found to be -5.46, -5.28; -2.26, -2.67; 3.20 and 2.61 eV, respectively. According to UV-Vis measurements, optical band gap （Eg） of 4-HBAP and P-4-HBAP were found to be 3.34 and 3.01 eV, respectively. Also, antimicrobial activities of 4-HBAP and P-4-HBAP were examined against selected some bacteria. The electrical conductivity of the polymer was measured after doping with iodine.
基金The study was funded by the Middle-Aged and Young Teachers in Colleges and Universities in Guangxi Basic Ability Promotion Project(No.2017KY0581)and Natural Science Foundation of Guangxi Province(No.2018GXNSFAA138140).
文摘The purpose of this study is to use the newly synthesized molecule Sodium 8-(((carboxymethyl)amino)methyl)-4',7-bishydroxy-isoflavone-3'-sulfonate(M)as a research object,the pharmacological mechanism of the molecule was analyzed by using a series of Systematic pharmacology methods.The results show that the M molecule has a higher drug-like DL value of 0.59 and better molecular property parameters,namely Hdon=4,Hacc=10 and AlogP=0.94;A total of 11 M molecules related targets,namely F2,ESR1,AR,F10,CA2,DPP4,CCNA2,PRSS1,CDK2,GSK3B and PTPN1;A total of 140 diseases are associated with M molecule targets,and these diseases are mainly related to cancer and cardiovascular diseases;A total of 52 pathways involve the pharmacological mechanisms of M molecules,which are mainly related to cancer and other related diseases;GO-enriched analysis showed that these targets are closely related to the regulation of peptidase activity and biological processes such as blood coagulation and hemostasis.This article clearly demonstrated the pharmacological mechanism of M molecule,which provides references for exploring the pharmacological mechanism of new compounds.
