The efficient separation of amphoteric organic compounds from dilute solutions is of great importance in the industrial field. In the present work, the reactive extractions of 4-hydroxypyridine(4-HP) with tributyl pho...The efficient separation of amphoteric organic compounds from dilute solutions is of great importance in the industrial field. In the present work, the reactive extractions of 4-hydroxypyridine(4-HP) with tributyl phosphate(TBP), di(2-ethylhexyl) phosphoric acid(D2EHPA) and TBP + D2EHPA dissolved in 1-octanol were investigated, respectively. The influences of the initial concentrations of TBP, D2EHPA and TBP + D2EHPA on distribution ratio(D) were discussed, as well as the reactive extraction mechanism were proposed. The obvious intensification effect was observed when the mixture of TBP and D2EHPA was used as extractant. The best extraction conditions were found to be of the molar ratio of D2EHPA and TBP at 2:1 and the equilibrium aqueous pH at 3.50-4.50. D values increased with the increase of the total concentration of TBP and D2EHPA in 1-octanol. Especially, the analysis on the extraction mechanisms clearly indicate(i) TBP in 1-octanol shows negligible reactive extraction toward 4-HP,(ii) D2EHPA in 1-octanol exhibits moderate extraction effect by forming 4-HP:D2EHPA(1:1) and 4-HP:2D2EHPA(1:2) type complexes, while(iii) D2EHPA in TBP/1-octanol demonstrates the maximum distribution ratio with the 4-HP:D2EHPA(1:1) type complex domination. The discussion provides new insights on the mechanism and opens a new way for the intensified extraction of amphoteric organic compounds by using the mixture of multiple extractants in the diluent.展开更多
This paper reports on the resolution of(R,S)-2-(4-methylphenyl)propionic acid(MPPA)enantiomers by enzymatic esterification in organic solvent.Novozym 435(CALB)has the best catalytic performance compared with other lip...This paper reports on the resolution of(R,S)-2-(4-methylphenyl)propionic acid(MPPA)enantiomers by enzymatic esterification in organic solvent.Novozym 435(CALB)has the best catalytic performance compared with other lipases.Of the alcohols screened,n-hexanol is the best acyl acceptor and gives the highest enzyme activity and enantioselectivity in n-hexane.Response surface methodology(RSM)was used to evaluate the influence of the factors,such as temperature,enzyme amount,substrate concentration and reaction time on the substrate conversion(c)and enantiomeric excess(ee).The correlation coefficient R2 for enantiomeric excess and the conversion are 0.9827 and 0.9910,respectively,indicating that can accurately predict the experimental results.By simulation and optimization,the optimal conditions were obtained,involving 600 mmol·L^-1 MPPA concentration(0.60 mmol),850 mmol·L^-1 hexanol concentration(0.85 mmol),58 mg enzyme amount,75℃temperature and 4.5 h reaction time,respectively.Under the optimized conditions,the experimental values of conversion and enantiomeric excess were 89.34%and 97.84%,respectively,which are in good agreement with the model predictions.展开更多
Six new transition metal complexes, [Zn(HBTC)(PYTPY)]n·n PYTPY(1), [Cu(HBTC)(PYTPY)]n·n PYTPY(2), [Co(HBTC)(PYTPY)]n·n DMF(3), [Mn(HBTC)(PYTPY)]n·n DMF(4), [Cd(HBTC)(PYTP...Six new transition metal complexes, [Zn(HBTC)(PYTPY)]n·n PYTPY(1), [Cu(HBTC)(PYTPY)]n·n PYTPY(2), [Co(HBTC)(PYTPY)]n·n DMF(3), [Mn(HBTC)(PYTPY)]n·n DMF(4), [Cd(HBTC)(PYTPY)(H2O)]n·2nH2O(5), and [Co(HBTC)(PYTPY)(H2O)2](6),(H3BTC = 1,3,5-benzenetricarboxylic acid, PYTPY = 4'-(4-pyridyl)-2,2':6',2''-terpyridine, DMF = N,N?-dimethylformamide), have been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. Complexes 1~5 all feature one-dimensional chain structures, and complex 6 exhibits a zero-dimensional structure. Complexes 1~5 present three-dimensional(3D) supramolecular frameworks via π-π stacking interactions, whenas 6 has also a 3D supramolecular structure assembled by hydrogen bonding. Meanwhile, complexes 1 ~ 6 exhibit the thermal stabilities and photoluminescent properties.展开更多
By using solvothermal method, two new metal coordination polymers based on 2,5-furandicarboxylic acid(H2FDA) ligand and 4,4'-bipyridine(bipy), [Cu(FDA)(4,4'-bipy)(DMF)]n·solvent(1) and {[Zn(4,4'-b...By using solvothermal method, two new metal coordination polymers based on 2,5-furandicarboxylic acid(H2FDA) ligand and 4,4'-bipyridine(bipy), [Cu(FDA)(4,4'-bipy)(DMF)]n·solvent(1) and {[Zn(4,4'-bipy)(FDA)(DMF)]·DMF}n(2), were produced and characterized by single-crystal X-ray diffraction analyses, elemental analyses, IR and powder X-ray diffraction. Compound 1 crystallizes in monoclinic space group P21/c with a = 11.104(2), b = 10.396(2), c = 18.772(4) , β = 96.20(3)o, V = 2154.2(7) 3, Dc = 1.378 g/cm^3, C19H17 Cu N3O6, Mr = 446.90, F(000) = 916, μ(Mo Kα) = 1.05 mm^-1, Z = 4, R = 0.0691 and wR = 0.1341 for 3537 observed reflections(I 2σ(I)), and R = 0.1062 and w R = 0.1482 for all data. Compound 2 crystallizes in monoclinic space group C2/c with a = 29.779(6), b = 9.6417(19), c = 17.292(3), β = 105.69(3)°, V = 4779.9(16) 3, Dc = 1.445 g/cm^3, C22H22N4O7 Zn, Mr = 519.81, F(000) = 2144, μ(Mo Kα)= 1.08 mm^-1, Z = 8, R = 0.0641 and w R = 0.1007 for 2985 observed reflections(I 2σ(I)), and R = 0.1028 and w R = 0.1112 for all data. Different coordination geometry of metal ions, square pyramid of Cu2+ and trigonal bipyramid of Zn2+, bring about different orientations of FDA2- ligands as well as 4,4'-bipyridine ligands, and furthermore distinct assembly structures for 1 and 2. The thermal stabilities of 1 and 2 are also investigated.展开更多
Two new metal-organic complexes [Cd2(1,4-BDC)(4-pytyp)(H2O)4]·(1,4-BDC)(1) and [Cu2(1,4-BDC)(4-pytyp)2(H2O)2]·(1,4-BDC)·8H2O(2)(4-pytyp = 4'-(4''-pyridyl)-2,2':6',2''-terp...Two new metal-organic complexes [Cd2(1,4-BDC)(4-pytyp)(H2O)4]·(1,4-BDC)(1) and [Cu2(1,4-BDC)(4-pytyp)2(H2O)2]·(1,4-BDC)·8H2O(2)(4-pytyp = 4'-(4''-pyridyl)-2,2':6',2''-terpyridine, 1,4-H2 BDC = 1,4-benzenedicarboxylic acid) have been synthesized under hydrothermal conditions and characterized by elemental analysis, infrared analysis and X-ray single-crystal diffraction. The scrutiny of single-crystal structure reveals that complex 1 forms to a 3D supramolecular network linked by π-π stacking interactions and hydrogen bonds. X-ray diffraction analysis reveals that complex 2 exhibits a 3D supramolecular network linked through complicated hydrogen bonds. The thermogravimetric analysis and photoluminescent properties of 1 and 2 are discussed in detail.展开更多
The title compound 4-(4,6-dimethoxylpyrimidin-2-yl)-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in eth...The title compound 4-(4,6-dimethoxylpyrimidin-2-yl)-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at the room temperature. The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis' Crystallographic data: C9H12N4O4S, Mr = 272.29, monoclinic, space group C2/m with a = 1.6672(3), b = 0.66383(12), c = 1.1617(2) nm, β = 109.275(2)°, V = 1.2136(4) nm^3, Dc = 1.490 g/cm^3,μ = 0.281 mm^-1, F(000) = 568, Z = 4, R1 = 0.0341and wR2 = 0.1042.展开更多
Racemic 2-n-butylbutanedioic acid 4-t-butyl esters were synthesized from methyl hexanoate and t-butyl α-iodoacetate via alkylation and subsequently selective hydrolyzation. The (R)-and (S)-2-n-butylbutanedioic ac...Racemic 2-n-butylbutanedioic acid 4-t-butyl esters were synthesized from methyl hexanoate and t-butyl α-iodoacetate via alkylation and subsequently selective hydrolyzation. The (R)-and (S)-2-n-butylbutanedioic acid 4-t-butyl esters were obtained by the resolution of the above-mentioned racemic compounds with(S)-( - ) or(R)-( + )-α- methylbenzylamine, respectively. The e.e. values of the two optical active products were determined to be above 99% by HPLC after the formation of two pairs of diastereoisomers with(R)-( + )-α-methylbenzylamine and(S)- phenylalanine methyl ester.展开更多
Chiral 4-[(2-isopropyl-5-methylcyclohexyl)oxo]-4-oxobutanoic acid reacts with substituted anilines to produce amides 1-6 in high yields. Resulted amides 1-6 were investigated for their antifungal and antibacterial act...Chiral 4-[(2-isopropyl-5-methylcyclohexyl)oxo]-4-oxobutanoic acid reacts with substituted anilines to produce amides 1-6 in high yields. Resulted amides 1-6 were investigated for their antifungal and antibacterial activities. Compounds 2 (96.5%) against Aspergillus fumigatus and 6 (93.7%) against Helminthosporium sativum demonstrated excellent activities. However, compounds 3 (37.6%) against Bacillus subtilis, 4 (33.2%) against Pseudomonas aurignosa, 5 against Klebsiella pneumonia demonstrated excellent growth inhibition potential.展开更多
4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single ...4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data: C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309(3), b = 0.67682(6), c = 1.74237(19) nm, β = 114.744(3)°, V= 2.7106(5) nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F(000) = 1200, Z= 8, R= 0.0514 and wR= 0.1529.展开更多
Two inorganic-organic coordination polymers, [Cd(TBA)2]·3H2O (1) and [Cu(TBA)2]·2H2O (2) have been synthesized by reaction of the metal ions of Cd(II) and Cu(II) with the ligand HTBA [HTBA = 4- (1H-1, 2, 4-t...Two inorganic-organic coordination polymers, [Cd(TBA)2]·3H2O (1) and [Cu(TBA)2]·2H2O (2) have been synthesized by reaction of the metal ions of Cd(II) and Cu(II) with the ligand HTBA [HTBA = 4- (1H-1, 2, 4-triazol-1-yl)benzoic acid] under solvothermal condition. The compounds were characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy, X-ray powder diffraction (XRPD), and thermo gravimetric analysis (TGA). The structural analyses reveal the two independent polymers exhibit different structures. Complex 1 exhibits a 3D framework with 1D channels, and complex 2 shows a 2-fold interpenetrating 3D diamond net.展开更多
<div style="text-align:justify;"> <span style="font-family:Verdana;">Medicinal plants have been used to treat many diseases with fewer side effects compared to clinical medicines. The n...<div style="text-align:justify;"> <span style="font-family:Verdana;">Medicinal plants have been used to treat many diseases with fewer side effects compared to clinical medicines. The need for treatment by medicinal plants has been increasing in response to the accumulation of environmental pollutants. The herbicide 2, 4-Dichlorophenoxyacetic acid has been considered as fast spreadable environmental pollutant, which may cause many disorders in animals and possibly in humans. The aim of this study is to assess the protective and/or curative effect of </span><i><span style="font-family:Verdana;">Lepidium sativum</span></i><span style="font-family:Verdana;"> against hepatotoxicity induced by 2, 4-D herbicide in rats. 25 Albino Wistar rats were grouped into 4 groups: a control group, the curative group treated for 4 weeks with LS water extract after a single dose 2, 4-D LD</span><sub><span style="font-family:Verdana;">50</span></sub><span style="font-family:Verdana;"> administration, protective group which was treated for 4 weeks with LS water extract prior to the 2, 4-D LD</span><sub><span style="font-family:Verdana;">50</span></sub><span style="font-family:Verdana;"> administration, and LS only group that was given the LS water extract as a positive control. Using transmission electron microscope, the histological features showed that curative group hepatocytes still suffered from focal necrosis and vacuolation of hepatocytes as a result of 2, 4-D toxic effect whereas in the protective group hepatocytes were less accentuated expressed as less frequent necrotic area, and still large mitochondria were present with numerous undissolved lipid droplets and a small amount of rough endoplasmic reticulum. For the LS only group, nearly normal cells with centric nucleus, normal small mitochondria were at a normal nucleus-cytoplasmic ratio, but a few lipid droplets were noticed. This study proved that curative group has an advantage over the protective group that could be presented in the nucleus with narrow nuclear pores and intact nuclear envelope with dense small mitochondria and normal rough endoplasmic reticulum that were recorded as in the control group. Thus, </span><i><span style="font-family:Verdana;">Lepidium sativum </span></i><span><span style="font-family:Verdana;">administration to the rats prior or post to intoxication was effective in minimizing the 2, 4-D-induced damages likely through a free radical scavenging activity in liver tissue.</span></span> </div>展开更多
A 3D coordination polymer [Zn2(hqc)2(H2O)]n has been obtained from the reaction of 4-hydroxyquinoline-2-carboxylic acid (H2hqc) with zinc(II) salt under hydrothermal condition, and characterized by elemental a...A 3D coordination polymer [Zn2(hqc)2(H2O)]n has been obtained from the reaction of 4-hydroxyquinoline-2-carboxylic acid (H2hqc) with zinc(II) salt under hydrothermal condition, and characterized by elemental analysis, IR, TGA, PXRD and X-ray single-crystal diffraction. The complex crystallizes in the monoclinic system, space group P21/c with a = 14.305(2), b = 9.132(2), c = 15.356(2), β = 103.586(7)o, V = 1949.9(4)3, Z = 4, Dc = 1.782 g/cm3, μ = 2.508 mm-1, Mr = 523.06, F(000) = 1048, T = 293(2) K, λ(MoKα) = 0.71073, S = 1.008, the final R = 0.0329 and wR = 0.0745 for 3849 observed reflections (I 〉 2σ(I)). The title complex features a 3D framework via Zn(2) linking the 1D {Zn1(hqc)2}n chains. Thermogravimetric analysis shows that its framework is highly thermally stable up to 556 ℃ in the solid state.展开更多
A new ID coordination polymer, [Cda(L1)2(L2)2].H2O (1, H2L1 = 4-(carboxy- methoxy)benzoic acid and L2 = 2-(4-fluorophenyl)-I H-imidazo[4,5-f][1,10]phenanthroline), has been hydrothermally synthesized and cha...A new ID coordination polymer, [Cda(L1)2(L2)2].H2O (1, H2L1 = 4-(carboxy- methoxy)benzoic acid and L2 = 2-(4-fluorophenyl)-I H-imidazo[4,5-f][1,10]phenanthroline), has been hydrothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.985(5), b = 10.768(5), c = 12.512(5) A, a = 68.959(5), β = 80.354(5), γ = 79.663(5)°, V= 1227.4(10) A3, Z = 1, C56H36Cd2F2N8O11, Mr = 1259.73, Dc = 1.704 g/cm3, F(000) = 630, μ(MoKa) = 0.949 mm-1, R = 0.0261 and wR = 0.0655. The L1 anions link the neighboring Cd(II) atoms to form a 1D double chain structure. The L2 ligands are alternately located on both sides of the double chains. More interestingly, the lateral L2 ligands from adjacent double chains are paired to furnish strong π-π interactions, yielding a 2D supramolecular layer. N-H...O, O-H...N and O-H...O hydrogen bonds further stabilize the structure of 1. The luminescent property of 1 was studied in solid state at room temperature.展开更多
The Ru3(CO)12/PEDPA complex was firstly applied in the CO selective reduction of 4-propylthio-2-mitroaniline. The effects of reaction temperature, the pressure of CO and concentration of catalyst on the reduction were...The Ru3(CO)12/PEDPA complex was firstly applied in the CO selective reduction of 4-propylthio-2-mitroaniline. The effects of reaction temperature, the pressure of CO and concentration of catalyst on the reduction were investigated. Under the optimum conditions of T=140℃, Pco=5.0MPa and substrate/catalyst = 300 (molar ratio), the conversion and selectivity were 70% and 98%, respectively. After simple phase separation, the catalyst could be recycled.展开更多
基金supported by the Science and Technology Research Project of Henan Province (192102310490 and 212102310505)。
文摘The efficient separation of amphoteric organic compounds from dilute solutions is of great importance in the industrial field. In the present work, the reactive extractions of 4-hydroxypyridine(4-HP) with tributyl phosphate(TBP), di(2-ethylhexyl) phosphoric acid(D2EHPA) and TBP + D2EHPA dissolved in 1-octanol were investigated, respectively. The influences of the initial concentrations of TBP, D2EHPA and TBP + D2EHPA on distribution ratio(D) were discussed, as well as the reactive extraction mechanism were proposed. The obvious intensification effect was observed when the mixture of TBP and D2EHPA was used as extractant. The best extraction conditions were found to be of the molar ratio of D2EHPA and TBP at 2:1 and the equilibrium aqueous pH at 3.50-4.50. D values increased with the increase of the total concentration of TBP and D2EHPA in 1-octanol. Especially, the analysis on the extraction mechanisms clearly indicate(i) TBP in 1-octanol shows negligible reactive extraction toward 4-HP,(ii) D2EHPA in 1-octanol exhibits moderate extraction effect by forming 4-HP:D2EHPA(1:1) and 4-HP:2D2EHPA(1:2) type complexes, while(iii) D2EHPA in TBP/1-octanol demonstrates the maximum distribution ratio with the 4-HP:D2EHPA(1:1) type complex domination. The discussion provides new insights on the mechanism and opens a new way for the intensified extraction of amphoteric organic compounds by using the mixture of multiple extractants in the diluent.
基金supported by the National Natural Science Foundation of China(21676077)。
文摘This paper reports on the resolution of(R,S)-2-(4-methylphenyl)propionic acid(MPPA)enantiomers by enzymatic esterification in organic solvent.Novozym 435(CALB)has the best catalytic performance compared with other lipases.Of the alcohols screened,n-hexanol is the best acyl acceptor and gives the highest enzyme activity and enantioselectivity in n-hexane.Response surface methodology(RSM)was used to evaluate the influence of the factors,such as temperature,enzyme amount,substrate concentration and reaction time on the substrate conversion(c)and enantiomeric excess(ee).The correlation coefficient R2 for enantiomeric excess and the conversion are 0.9827 and 0.9910,respectively,indicating that can accurately predict the experimental results.By simulation and optimization,the optimal conditions were obtained,involving 600 mmol·L^-1 MPPA concentration(0.60 mmol),850 mmol·L^-1 hexanol concentration(0.85 mmol),58 mg enzyme amount,75℃temperature and 4.5 h reaction time,respectively.Under the optimized conditions,the experimental values of conversion and enantiomeric excess were 89.34%and 97.84%,respectively,which are in good agreement with the model predictions.
基金Supported by the National Natural Science Foundation of China(No.21576112)Natural Science Foundation of Jilin Province(20150623024TC-19,20170520147JH)the Science and Technology Development Plan of Siping City(2015049)
文摘Six new transition metal complexes, [Zn(HBTC)(PYTPY)]n·n PYTPY(1), [Cu(HBTC)(PYTPY)]n·n PYTPY(2), [Co(HBTC)(PYTPY)]n·n DMF(3), [Mn(HBTC)(PYTPY)]n·n DMF(4), [Cd(HBTC)(PYTPY)(H2O)]n·2nH2O(5), and [Co(HBTC)(PYTPY)(H2O)2](6),(H3BTC = 1,3,5-benzenetricarboxylic acid, PYTPY = 4'-(4-pyridyl)-2,2':6',2''-terpyridine, DMF = N,N?-dimethylformamide), have been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. Complexes 1~5 all feature one-dimensional chain structures, and complex 6 exhibits a zero-dimensional structure. Complexes 1~5 present three-dimensional(3D) supramolecular frameworks via π-π stacking interactions, whenas 6 has also a 3D supramolecular structure assembled by hydrogen bonding. Meanwhile, complexes 1 ~ 6 exhibit the thermal stabilities and photoluminescent properties.
基金supported by URT program of Beijing Institute of Petrochemical Technology(Beijing municipal level 2015J00058)URT program of Beijing Institute of Petrochemical Technology(State level 2015J00056)
文摘By using solvothermal method, two new metal coordination polymers based on 2,5-furandicarboxylic acid(H2FDA) ligand and 4,4'-bipyridine(bipy), [Cu(FDA)(4,4'-bipy)(DMF)]n·solvent(1) and {[Zn(4,4'-bipy)(FDA)(DMF)]·DMF}n(2), were produced and characterized by single-crystal X-ray diffraction analyses, elemental analyses, IR and powder X-ray diffraction. Compound 1 crystallizes in monoclinic space group P21/c with a = 11.104(2), b = 10.396(2), c = 18.772(4) , β = 96.20(3)o, V = 2154.2(7) 3, Dc = 1.378 g/cm^3, C19H17 Cu N3O6, Mr = 446.90, F(000) = 916, μ(Mo Kα) = 1.05 mm^-1, Z = 4, R = 0.0691 and wR = 0.1341 for 3537 observed reflections(I 2σ(I)), and R = 0.1062 and w R = 0.1482 for all data. Compound 2 crystallizes in monoclinic space group C2/c with a = 29.779(6), b = 9.6417(19), c = 17.292(3), β = 105.69(3)°, V = 4779.9(16) 3, Dc = 1.445 g/cm^3, C22H22N4O7 Zn, Mr = 519.81, F(000) = 2144, μ(Mo Kα)= 1.08 mm^-1, Z = 8, R = 0.0641 and w R = 0.1007 for 2985 observed reflections(I 2σ(I)), and R = 0.1028 and w R = 0.1112 for all data. Different coordination geometry of metal ions, square pyramid of Cu2+ and trigonal bipyramid of Zn2+, bring about different orientations of FDA2- ligands as well as 4,4'-bipyridine ligands, and furthermore distinct assembly structures for 1 and 2. The thermal stabilities of 1 and 2 are also investigated.
基金Supported by the Program for New Century Excellent Talents in University(NCET-10-0176)the Natural Science Foundation of Jilin Province(No.20130521019JH)the fund of Jilin Provincial Education Department of China(No.2014154)
文摘Two new metal-organic complexes [Cd2(1,4-BDC)(4-pytyp)(H2O)4]·(1,4-BDC)(1) and [Cu2(1,4-BDC)(4-pytyp)2(H2O)2]·(1,4-BDC)·8H2O(2)(4-pytyp = 4'-(4''-pyridyl)-2,2':6',2''-terpyridine, 1,4-H2 BDC = 1,4-benzenedicarboxylic acid) have been synthesized under hydrothermal conditions and characterized by elemental analysis, infrared analysis and X-ray single-crystal diffraction. The scrutiny of single-crystal structure reveals that complex 1 forms to a 3D supramolecular network linked by π-π stacking interactions and hydrogen bonds. X-ray diffraction analysis reveals that complex 2 exhibits a 3D supramolecular network linked through complicated hydrogen bonds. The thermogravimetric analysis and photoluminescent properties of 1 and 2 are discussed in detail.
基金This work was supported by the National Natural Science Foundation of China (20571060) and Education Committee of Shaan Xi Province (05JK294)
文摘The title compound 4-(4,6-dimethoxylpyrimidin-2-yl)-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at the room temperature. The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis' Crystallographic data: C9H12N4O4S, Mr = 272.29, monoclinic, space group C2/m with a = 1.6672(3), b = 0.66383(12), c = 1.1617(2) nm, β = 109.275(2)°, V = 1.2136(4) nm^3, Dc = 1.490 g/cm^3,μ = 0.281 mm^-1, F(000) = 568, Z = 4, R1 = 0.0341and wR2 = 0.1042.
基金Supported by the National Basic Research Priority Program(No. 2003CCA027).
文摘Racemic 2-n-butylbutanedioic acid 4-t-butyl esters were synthesized from methyl hexanoate and t-butyl α-iodoacetate via alkylation and subsequently selective hydrolyzation. The (R)-and (S)-2-n-butylbutanedioic acid 4-t-butyl esters were obtained by the resolution of the above-mentioned racemic compounds with(S)-( - ) or(R)-( + )-α- methylbenzylamine, respectively. The e.e. values of the two optical active products were determined to be above 99% by HPLC after the formation of two pairs of diastereoisomers with(R)-( + )-α-methylbenzylamine and(S)- phenylalanine methyl ester.
文摘Chiral 4-[(2-isopropyl-5-methylcyclohexyl)oxo]-4-oxobutanoic acid reacts with substituted anilines to produce amides 1-6 in high yields. Resulted amides 1-6 were investigated for their antifungal and antibacterial activities. Compounds 2 (96.5%) against Aspergillus fumigatus and 6 (93.7%) against Helminthosporium sativum demonstrated excellent activities. However, compounds 3 (37.6%) against Bacillus subtilis, 4 (33.2%) against Pseudomonas aurignosa, 5 against Klebsiella pneumonia demonstrated excellent growth inhibition potential.
基金supported by the National Natural Science Foundation of China (20571060)Natural Science Foundation of Shaanxi Province (2007B08)Education Committee of Shaanxi Province (05JK294)
文摘4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data: C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309(3), b = 0.67682(6), c = 1.74237(19) nm, β = 114.744(3)°, V= 2.7106(5) nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F(000) = 1200, Z= 8, R= 0.0514 and wR= 0.1529.
文摘Two inorganic-organic coordination polymers, [Cd(TBA)2]·3H2O (1) and [Cu(TBA)2]·2H2O (2) have been synthesized by reaction of the metal ions of Cd(II) and Cu(II) with the ligand HTBA [HTBA = 4- (1H-1, 2, 4-triazol-1-yl)benzoic acid] under solvothermal condition. The compounds were characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy, X-ray powder diffraction (XRPD), and thermo gravimetric analysis (TGA). The structural analyses reveal the two independent polymers exhibit different structures. Complex 1 exhibits a 3D framework with 1D channels, and complex 2 shows a 2-fold interpenetrating 3D diamond net.
文摘<div style="text-align:justify;"> <span style="font-family:Verdana;">Medicinal plants have been used to treat many diseases with fewer side effects compared to clinical medicines. The need for treatment by medicinal plants has been increasing in response to the accumulation of environmental pollutants. The herbicide 2, 4-Dichlorophenoxyacetic acid has been considered as fast spreadable environmental pollutant, which may cause many disorders in animals and possibly in humans. The aim of this study is to assess the protective and/or curative effect of </span><i><span style="font-family:Verdana;">Lepidium sativum</span></i><span style="font-family:Verdana;"> against hepatotoxicity induced by 2, 4-D herbicide in rats. 25 Albino Wistar rats were grouped into 4 groups: a control group, the curative group treated for 4 weeks with LS water extract after a single dose 2, 4-D LD</span><sub><span style="font-family:Verdana;">50</span></sub><span style="font-family:Verdana;"> administration, protective group which was treated for 4 weeks with LS water extract prior to the 2, 4-D LD</span><sub><span style="font-family:Verdana;">50</span></sub><span style="font-family:Verdana;"> administration, and LS only group that was given the LS water extract as a positive control. Using transmission electron microscope, the histological features showed that curative group hepatocytes still suffered from focal necrosis and vacuolation of hepatocytes as a result of 2, 4-D toxic effect whereas in the protective group hepatocytes were less accentuated expressed as less frequent necrotic area, and still large mitochondria were present with numerous undissolved lipid droplets and a small amount of rough endoplasmic reticulum. For the LS only group, nearly normal cells with centric nucleus, normal small mitochondria were at a normal nucleus-cytoplasmic ratio, but a few lipid droplets were noticed. This study proved that curative group has an advantage over the protective group that could be presented in the nucleus with narrow nuclear pores and intact nuclear envelope with dense small mitochondria and normal rough endoplasmic reticulum that were recorded as in the control group. Thus, </span><i><span style="font-family:Verdana;">Lepidium sativum </span></i><span><span style="font-family:Verdana;">administration to the rats prior or post to intoxication was effective in minimizing the 2, 4-D-induced damages likely through a free radical scavenging activity in liver tissue.</span></span> </div>
基金supported by 973 (2011CB932504)NNSFC (20971121)NSF of Fujian Province
文摘A 3D coordination polymer [Zn2(hqc)2(H2O)]n has been obtained from the reaction of 4-hydroxyquinoline-2-carboxylic acid (H2hqc) with zinc(II) salt under hydrothermal condition, and characterized by elemental analysis, IR, TGA, PXRD and X-ray single-crystal diffraction. The complex crystallizes in the monoclinic system, space group P21/c with a = 14.305(2), b = 9.132(2), c = 15.356(2), β = 103.586(7)o, V = 1949.9(4)3, Z = 4, Dc = 1.782 g/cm3, μ = 2.508 mm-1, Mr = 523.06, F(000) = 1048, T = 293(2) K, λ(MoKα) = 0.71073, S = 1.008, the final R = 0.0329 and wR = 0.0745 for 3849 observed reflections (I 〉 2σ(I)). The title complex features a 3D framework via Zn(2) linking the 1D {Zn1(hqc)2}n chains. Thermogravimetric analysis shows that its framework is highly thermally stable up to 556 ℃ in the solid state.
基金Supported by Jilin Province Science and Technology Development projects (No. 201105085)
文摘A new ID coordination polymer, [Cda(L1)2(L2)2].H2O (1, H2L1 = 4-(carboxy- methoxy)benzoic acid and L2 = 2-(4-fluorophenyl)-I H-imidazo[4,5-f][1,10]phenanthroline), has been hydrothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.985(5), b = 10.768(5), c = 12.512(5) A, a = 68.959(5), β = 80.354(5), γ = 79.663(5)°, V= 1227.4(10) A3, Z = 1, C56H36Cd2F2N8O11, Mr = 1259.73, Dc = 1.704 g/cm3, F(000) = 630, μ(MoKa) = 0.949 mm-1, R = 0.0261 and wR = 0.0655. The L1 anions link the neighboring Cd(II) atoms to form a 1D double chain structure. The L2 ligands are alternately located on both sides of the double chains. More interestingly, the lateral L2 ligands from adjacent double chains are paired to furnish strong π-π interactions, yielding a 2D supramolecular layer. N-H...O, O-H...N and O-H...O hydrogen bonds further stabilize the structure of 1. The luminescent property of 1 was studied in solid state at room temperature.
文摘The Ru3(CO)12/PEDPA complex was firstly applied in the CO selective reduction of 4-propylthio-2-mitroaniline. The effects of reaction temperature, the pressure of CO and concentration of catalyst on the reduction were investigated. Under the optimum conditions of T=140℃, Pco=5.0MPa and substrate/catalyst = 300 (molar ratio), the conversion and selectivity were 70% and 98%, respectively. After simple phase separation, the catalyst could be recycled.