Under mild conditions, conversion of a variety of ketoximes and aldoximes to their corresponding amides and nitriles proceeded in the presence of PEG-SO3H with high yields.
The crystal structure of the title compound (C18H18N4O, Mr = 306.36) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with α = 4.783(0), b = 13.577(1), c = 13...The crystal structure of the title compound (C18H18N4O, Mr = 306.36) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with α = 4.783(0), b = 13.577(1), c = 13.830(1) A, α = 63.581(2), β = 88.326(2), γ = 86.161(2)°, V= 802.5(1) A3, Z= 2, Dc = 1.268 g/cm^3, F(000) = 324, μ(MoKa) = 0.082 mm^-1, the final R = 0.0497 and wR = 0.1199 for 3094 observed reflections (I 〉 2σ(I)). The dihedral angles between the phenyl (C(1)-C(4)-(6)) and triazole, the phenyl (C(13)-C(15)-C(18)) and triazole, and the two phenyl rings are 7.9(1), 69.9(1) and 67.8(1)°, respectively. Strong C-H…π interaction joins molecules into a chain along the c axis and contributes to the stability of the structure. Preliminary bioassay results show that the title compound possesses excellent and selective fungicidal activity against Colletotrichum gossypii but displays moderate to weak insecticidal activity against aphides.展开更多
A pair of E/Z-isomers of 2-phenyl-6,7-dihydrobenzofuran-4(5H)-one O-cyanomethyl oxime,C16H14N2O2,as potential drugs for treating peptic ulcer and other acid-related diseases have been synthesized and characterized b...A pair of E/Z-isomers of 2-phenyl-6,7-dihydrobenzofuran-4(5H)-one O-cyanomethyl oxime,C16H14N2O2,as potential drugs for treating peptic ulcer and other acid-related diseases have been synthesized and characterized by IR,MS and NMR spectra.Meanwhile,the crystal of IIIa was obtained and determined by X-ray single-crystal diffraction.Crystal data: monoclinic system,space group P21 /c,a = 8.423(8),b = 19.596(16),c = 8.770(8),β = 107.750(12)°,V = 1379(2)3,Z = 4,F(000) = 560,Dc = 1.283 g/cm3,μ = 0.086 mm 1,R = 0.0681 and wR = 0.2029 for 14472 independent reflections(Rint = 0.0782) and 2428 observed ones(I 2σ(I)).展开更多
The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65~68% HNO3. Its crystal structure was determin...The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65~68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481(8), b = 9.3351(5), c = 13.1911(7) , β = 98.9450(10)°, Z = 4, V = 1769.67(17) 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F(000) = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections (I 2σ(I)). X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.展开更多
Acetophenone oxime and benzaldehyde oxime were converted to oxime ethers in the presence of alkyl halide or methyl sulfate and KOH in aqueous DMSO in 5 to 70 min. The yields of oxime ethers were 70 - 96%.
A convenient synthesis of 1-alkyl-2-chloro-1H-indole-3-carbaldehyde oximes(5a―5d) and 1-alkyl-2-phenoxy-1H-indole-3-carbaldehyde oximes(6a―6d) from 2-indolone was completed via the Vilsmeier-Haack reac-tion,with...A convenient synthesis of 1-alkyl-2-chloro-1H-indole-3-carbaldehyde oximes(5a―5d) and 1-alkyl-2-phenoxy-1H-indole-3-carbaldehyde oximes(6a―6d) from 2-indolone was completed via the Vilsmeier-Haack reac-tion,with N-alkylation and oximation as the key steps.An improved one-pot method for the synthesis of 1-alkyl-2-alkoxy-1H-indole-3-carbaldehyde oximes(7a―7h) from 1-alkyl-2-chloro-1H-indole-3-carbaldehydes(3a―3d) was described.The Williamson reactions and esterification reactions were performed and the oxime-ethers and oxime-esters were synthesized,respectively.The new synthesized compounds(3a―11d) were characterized by 1H NMR,IR,MS,and elemental analysis.展开更多
Three novel dehydroabietate oxime derivatives were synthesized from dehydroabietic acid and their crystal structures were determined by X-ray crystallographic techniques. All of these 12-oxime dehydroabietic acid deri...Three novel dehydroabietate oxime derivatives were synthesized from dehydroabietic acid and their crystal structures were determined by X-ray crystallographic techniques. All of these 12-oxime dehydroabietic acid derivatives crystallize in orthorhombic system, space group P212121. In the structures, rings A and B exhibit chair and half-chair configurations, respectively and form trans ring junction with two methyl groups(C(19) and C(20)) in the axis positions. The oxime groups have E conformations. Comparison of conformations reveals subtle differences principally in ring B due to the modification in C(12). The E-acetaldehyde oxime derivative 2c showed distinct BKα gate-opening activity with an ionic current increase of 164% at 30 μM versus the control current.展开更多
Dioxane-NO2 was employed to oxidize oximes to corresponding aldehydes and ketones in high yield in nonaqueous condition at room temperature. Thr reaction proved to be mild and selective.
Two manganese complexes, [Mn3(2-cba)6(phen)2] 1 (2-cba = 2-cyanobenzoic acid, phe11 = 1,10-phenanthroline) and [MnE(4-fbaO)E(phen)4](PF6)E.EHEO 2 (4-fbao = 4-formylbenzoic acid oxime), have been synthesi...Two manganese complexes, [Mn3(2-cba)6(phen)2] 1 (2-cba = 2-cyanobenzoic acid, phe11 = 1,10-phenanthroline) and [MnE(4-fbaO)E(phen)4](PF6)E.EHEO 2 (4-fbao = 4-formylbenzoic acid oxime), have been synthesized by the reaction of 2-formylbenzoic acid oxime (2-fbao, HELl) or 4-formylbenzoic acid oxime (4-fbao, HELE) with phen and manganese acetate in ethanol or methanol solution. A translation from the oximino (-CHN=OH) of HELl to cyano (-C-N) was found in the formation of complex 1 at room temperature. The complexes were structurally determined by single-crystal X-ray diffraction. The crystal of compound I belongs to monoclinic, space group C2/c, with a = 17.983(6), b = 23.364(7), c =14.589(5) A, β = 92.401(5)° V = 6124(3) A^3, Z = 4, C72H40Mn3N10O12, Mr= 1401.96, Dc = 1.521 g/cm^3, F(000) = 2852.0, Rint = 0.0372, T= 293(2) K,μ = 0.686 mm^-1, the final R = 0.0644 and wR = 0.1813 for 5803 observed reflections with I 〉 2δ(I). The crystal of compound 2 is of monoclinic system, space group P21/n, with a = 13.050(4), b = 20.577(5), c = 13.323(4)A,β = 113.578(3)°, V = 3227.2(14)A3, Z = 2, C64H48F12Mn2N10O8P2, Mr = 1484.94, Dc = 1.528 g/cm^3, F(000) = 1508.0, Rint= 0.0295, T= 293(2) K,μ = 0.539 mm^-1, the final R = 0.0629 and wR = 0.1789 for 5298 observed reflections with I 〉 2σ(I). Compounds 1 and 2 are linear trinuclear and dinuclear manganese complexes respectively, which are both bridged by carboxylate groups of the ligands.展开更多
The title complex, C18H15N3NiO3, has been prepared and characterized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group Cc with a = 10.939(2), b = 22.909(5), c = 6.907(1) ?, β = 11...The title complex, C18H15N3NiO3, has been prepared and characterized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group Cc with a = 10.939(2), b = 22.909(5), c = 6.907(1) ?, β = 116.75(3)°, V = 1545.7(5) ?, Z = 4, Mr = 380.04, F(000) = 784, Dc = 1.633 g/cm3 and μ(MoKα) = 1.279 mm–1. The structure was refined to R = 0.0472 and wR = 0.0893 for 2571 observed reflections with I > 2σ(I). The absolute structure Flack parameter X is 0.01(2). In this crystal structure, strong face-to-face π-π stacking interactions between adjacent molecules lead to a one-dimensional chain structure.展开更多
The comparative process for preparing 9-oxime erythromycin A (EMAO) is investigated. EMAO was synthesized and compared by the reaction of erythromycin and hydroxylamine hydrochloride with various bases such as sodium...The comparative process for preparing 9-oxime erythromycin A (EMAO) is investigated. EMAO was synthesized and compared by the reaction of erythromycin and hydroxylamine hydrochloride with various bases such as sodium acetate, triethylamine, etc. A new synthetic method is established. The oximation is performed under dynamic buffer system; less degradation impurities are formed. The yield of EMAO reaches more than 95%, HPLC analysis shows that the purity of EMAO is more than 90%, and the E/Z isomeric ratio preponderates over 7∶1.展开更多
The Beckmann rearrangement of cyclohexanone oxime was achieved by the combined use of cobalt salt and Lewis acids co-catalysts (each 10 mol%). Various combinations of cobalt salts and Lewis acids gave lactams in a sat...The Beckmann rearrangement of cyclohexanone oxime was achieved by the combined use of cobalt salt and Lewis acids co-catalysts (each 10 mol%). Various combinations of cobalt salts and Lewis acids gave lactams in a satisfactory yield under mild conditions. This method makes it possible to reduce undesirable byproducts.展开更多
A series of novel flavone-4-oximes[1]were synthesized by the oximation of substituted flavones.The synthesized compounds were characterized by various spectroscopic methods including IR,MASS,NMR spectroscopy.Out of th...A series of novel flavone-4-oximes[1]were synthesized by the oximation of substituted flavones.The synthesized compounds were characterized by various spectroscopic methods including IR,MASS,NMR spectroscopy.Out of the 14 test compounds screened for their antioxidant activity,compounds such as JGS-VI(a N,N dimethyl benzaldehyde derivative)and JGSVII(a 3,4 dimethoxy benzaldehyde derivative)exhibited antioxidant activity comparable to that of ascorbic acid with its IC50 value at 30.01 Mm as standard following DPPH?method.Compounds such as JGS-II(a Para fluro benzaldehyde derivative),JGS-IV(a Para methyl benzaldehyde derivative)and JGS-V(a thiophene-2-aldehyde derivative)exhibited anti-oxidant activity among all the test compounds screened against ABTS[2]using Quercetin with its IC50 value at 50.24 Mm.展开更多
The synthesis of two new methacrylates such as 2-[(cyclohexylideneamino)oxy]-2-oxoethyl methylacrylate (CHOEMA)and 2-[(cyclopentylideneamino)oxy]-2-oxoethyl methylacrylate(CPOEMA)are described.The monomers produced fr...The synthesis of two new methacrylates such as 2-[(cyclohexylideneamino)oxy]-2-oxoethyl methylacrylate (CHOEMA)and 2-[(cyclopentylideneamino)oxy]-2-oxoethyl methylacrylate(CPOEMA)are described.The monomers produced from the reaction of corresponding cyclohexanone O-(2-chloroacetyl)oxime and cyclopentanone O-(2- chloroacetyl)oxime with sodium methacrylate was polymerized in 1,4-dioxane solution at 65℃using AIBN as an initiator. The monomers and their polymers were characterized by IR,~1H- and ^(13)C-NMR spec...展开更多
The addition of platinum over the B2O3/TiO2-ZrO2 remarkably enhanced its catalytic stability in the vapor phase Beckmann rearrangement of cyclohexanone oxime under the carder gas of H2. The content of coke deposited ...The addition of platinum over the B2O3/TiO2-ZrO2 remarkably enhanced its catalytic stability in the vapor phase Beckmann rearrangement of cyclohexanone oxime under the carder gas of H2. The content of coke deposited on catalyst surface was decreased from 1.92% over the B2O3/TiO2-ZrO2 to 1.14% over the platinum promoted B2O3/TiO2-ZrO2 after reaction of six hours. This result indicates that the platinum added on the B2O3/TiO2-ZrO2 catalyst plays an important role in reducing the coke formation on the catalyst surface.展开更多
The pharmacokinetics of milbemycin oxime was investigated in dogs following oral(per os, PO) and intravenous(IV) administration. Three groups of dogs received milbemycin oxime tablets as a single PO dose equal to 0.25...The pharmacokinetics of milbemycin oxime was investigated in dogs following oral(per os, PO) and intravenous(IV) administration. Three groups of dogs received milbemycin oxime tablets as a single PO dose equal to 0.25, 0.5 and 1.0 mg · kg-1 of milbemycin oxime, respectively, another group received a single IV dose of 0.5 mg · kg-1. Blood samples were collected at predetermined times after drug administration and the milbemycin oxime concentrations in plasma were determined by LC-MS/MS. The drug protein binding in dog plasma in vitro was determined by equilibrium dialysis at concentrations spanning the range of values observed in vivo in dog plasma. After PO administration at doses of 0.25, 0.5 and 1.0 mg · kg-1, milbemycin oxime was slowly absorbed and eliminated, the time to reach the maximum plasma concentration(Tmax) was 4.14±0.20, 4.27±0.14 and 4.06±0.13 h, the mean absorption time(MAT) was 19.06, 13.67 and 11.77 h, the terminal rate half-life(t1/2λz) was 15.06±0.37, 11.09±0.54 and 9.76±0.89 h and the total body clearance(Cl) was 1.15±0.05, 1.18±0.03 and 1.17±0.07 m L · min-1 · kg-1, respectively. The maximum plasma concentration(Cmax, 36.50±1.40, 76.11±2.77 and 182.05±7.20 ng · m L-1, respectively) and the area under the first-moment curve(AUC-10→∞, 985.83±49.46, 1 663.12±51.42 and 3 558.04±197.88 mg · h · L, respectively) increased accordingly to the administered dose rates; the oral bioavailabilities were estimated to be 88.61%, 74.75% and 79.96%, respectively. The values of fu were 0.12%, 0.14% and 0.13% in dog plasma, respectively. In conclusion, the pharmacokinetics of milbemycin oxime in dogs following oral administration revealed its higher oral bioavailability and advantageous pharmacokinetic properties, such as its lower total body clearance and longer elimination half-life, and indicated that the single oral dose of 0.50 mg · kg-1 of milbemycin oxime which was recommended in all the parasitological efficacy studies allowed an adequate concentration of the drug.展开更多
A novel derivative of glycyrrhetinic acid, (E)-ethyl 3-keto-18β-glycyrrhetinate 3- oxime C32H49NO4 (Mr = 511.72), was synthesized and structurally characterized by IR, 1^H NMR and single-crystal X-ray diffraction...A novel derivative of glycyrrhetinic acid, (E)-ethyl 3-keto-18β-glycyrrhetinate 3- oxime C32H49NO4 (Mr = 511.72), was synthesized and structurally characterized by IR, 1^H NMR and single-crystal X-ray diffraction. It belongs to monoclinic, space group P21, with a = 12.4897(12), b = 7.3190(7), c = 15.9944(14)A, β = 94.833(2)o, V = 1456.9(2)A^3, Z = 2, Dc = 1.167 g/cm^3, μ = 0.075 mm^-1, F(000) = 560, the final R = 0.0449 and wR = 0.1122. A total of 7486 reflections were collected, of which 2785 were independent (Rint = 0.0199) and 2605 were observed with I 〉 2σ(I). There exists an intermolecular hydrogen bond which helps to stabilize the crystal structure.展开更多
Eleven new 1-{5-[4-(benzyloxy)phenyl]-3-methyl-4,5-dihydropyrazol-l-yl} oxime ester dcrivatives were synthesized and characterized by elemental analysis, HRMS, ^1H NMR data. All the compounds were screened for their...Eleven new 1-{5-[4-(benzyloxy)phenyl]-3-methyl-4,5-dihydropyrazol-l-yl} oxime ester dcrivatives were synthesized and characterized by elemental analysis, HRMS, ^1H NMR data. All the compounds were screened for their antibacterial potential in vitro against Bacillus subtilis, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa. The results indicate that compounds 8c and 8f possess potent activity with the minimum inhibitory concentrations(MIC) of 1.562--3.125 ug/mL against all the four bacteria. Compounds 8c, 8e and 8f show moderate inhibition against the DNA gyrase(IC50=1.9--2.5 ug/mL). On the basis of the biological activities, structure-activity relationship was discussed.展开更多
基金support from the Natural Science Foundation of Gansu Province(No.3ZS061-A25-019)the Scientific Research fund of Gansu Provincial Education Department(No.0601-25)
文摘Under mild conditions, conversion of a variety of ketoximes and aldoximes to their corresponding amides and nitriles proceeded in the presence of PEG-SO3H with high yields.
基金Supported by NNSFC (20302002 and 20872046)the SRF for ROCS, SEM (No. [2007] 1108)
文摘The crystal structure of the title compound (C18H18N4O, Mr = 306.36) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with α = 4.783(0), b = 13.577(1), c = 13.830(1) A, α = 63.581(2), β = 88.326(2), γ = 86.161(2)°, V= 802.5(1) A3, Z= 2, Dc = 1.268 g/cm^3, F(000) = 324, μ(MoKa) = 0.082 mm^-1, the final R = 0.0497 and wR = 0.1199 for 3094 observed reflections (I 〉 2σ(I)). The dihedral angles between the phenyl (C(1)-C(4)-(6)) and triazole, the phenyl (C(13)-C(15)-C(18)) and triazole, and the two phenyl rings are 7.9(1), 69.9(1) and 67.8(1)°, respectively. Strong C-H…π interaction joins molecules into a chain along the c axis and contributes to the stability of the structure. Preliminary bioassay results show that the title compound possesses excellent and selective fungicidal activity against Colletotrichum gossypii but displays moderate to weak insecticidal activity against aphides.
基金Supported by the National Natural Science Foundation of China(Nos.21102084,21272136,31070313)Scientific and Technological Research Project of Hubei Provincial Department of Education(No.Q20111210)Science Foundation of China Three Gorges University(No.KJ2010B001)
文摘A pair of E/Z-isomers of 2-phenyl-6,7-dihydrobenzofuran-4(5H)-one O-cyanomethyl oxime,C16H14N2O2,as potential drugs for treating peptic ulcer and other acid-related diseases have been synthesized and characterized by IR,MS and NMR spectra.Meanwhile,the crystal of IIIa was obtained and determined by X-ray single-crystal diffraction.Crystal data: monoclinic system,space group P21 /c,a = 8.423(8),b = 19.596(16),c = 8.770(8),β = 107.750(12)°,V = 1379(2)3,Z = 4,F(000) = 560,Dc = 1.283 g/cm3,μ = 0.086 mm 1,R = 0.0681 and wR = 0.2029 for 14472 independent reflections(Rint = 0.0782) and 2428 observed ones(I 2σ(I)).
基金Supported by the Central University Basic Scientific Research Fund of Hunan University (2009)the Key Scientific and Technological Project of Changsha, Hunan Province (No. 0901077-31)
文摘The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65~68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481(8), b = 9.3351(5), c = 13.1911(7) , β = 98.9450(10)°, Z = 4, V = 1769.67(17) 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F(000) = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections (I 2σ(I)). X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.
文摘Acetophenone oxime and benzaldehyde oxime were converted to oxime ethers in the presence of alkyl halide or methyl sulfate and KOH in aqueous DMSO in 5 to 70 min. The yields of oxime ethers were 70 - 96%.
基金Supported by the Natural Science Foundation of Liaoning Province,China(No.202142037)
文摘A convenient synthesis of 1-alkyl-2-chloro-1H-indole-3-carbaldehyde oximes(5a―5d) and 1-alkyl-2-phenoxy-1H-indole-3-carbaldehyde oximes(6a―6d) from 2-indolone was completed via the Vilsmeier-Haack reac-tion,with N-alkylation and oximation as the key steps.An improved one-pot method for the synthesis of 1-alkyl-2-alkoxy-1H-indole-3-carbaldehyde oximes(7a―7h) from 1-alkyl-2-chloro-1H-indole-3-carbaldehydes(3a―3d) was described.The Williamson reactions and esterification reactions were performed and the oxime-ethers and oxime-esters were synthesized,respectively.The new synthesized compounds(3a―11d) were characterized by 1H NMR,IR,MS,and elemental analysis.
基金supports from the National Natural Science Foundation of China (No. 81202402 and 21272154)
文摘Three novel dehydroabietate oxime derivatives were synthesized from dehydroabietic acid and their crystal structures were determined by X-ray crystallographic techniques. All of these 12-oxime dehydroabietic acid derivatives crystallize in orthorhombic system, space group P212121. In the structures, rings A and B exhibit chair and half-chair configurations, respectively and form trans ring junction with two methyl groups(C(19) and C(20)) in the axis positions. The oxime groups have E conformations. Comparison of conformations reveals subtle differences principally in ring B due to the modification in C(12). The E-acetaldehyde oxime derivative 2c showed distinct BKα gate-opening activity with an ionic current increase of 164% at 30 μM versus the control current.
基金the National Natural Science Foundation of China and Henan Province Education Committee.
文摘Dioxane-NO2 was employed to oxidize oximes to corresponding aldehydes and ketones in high yield in nonaqueous condition at room temperature. Thr reaction proved to be mild and selective.
基金grants from the 973 Program (2007CB815301 and 2006CB932900)the National Natural Science Foundation of China (20733003 and 20673118)+1 种基金the Science Foundation of CAS (KJCX2-YW-M05)Fujian Province (2006F3132 and 2005HZ01-1)
文摘Two manganese complexes, [Mn3(2-cba)6(phen)2] 1 (2-cba = 2-cyanobenzoic acid, phe11 = 1,10-phenanthroline) and [MnE(4-fbaO)E(phen)4](PF6)E.EHEO 2 (4-fbao = 4-formylbenzoic acid oxime), have been synthesized by the reaction of 2-formylbenzoic acid oxime (2-fbao, HELl) or 4-formylbenzoic acid oxime (4-fbao, HELE) with phen and manganese acetate in ethanol or methanol solution. A translation from the oximino (-CHN=OH) of HELl to cyano (-C-N) was found in the formation of complex 1 at room temperature. The complexes were structurally determined by single-crystal X-ray diffraction. The crystal of compound I belongs to monoclinic, space group C2/c, with a = 17.983(6), b = 23.364(7), c =14.589(5) A, β = 92.401(5)° V = 6124(3) A^3, Z = 4, C72H40Mn3N10O12, Mr= 1401.96, Dc = 1.521 g/cm^3, F(000) = 2852.0, Rint = 0.0372, T= 293(2) K,μ = 0.686 mm^-1, the final R = 0.0644 and wR = 0.1813 for 5803 observed reflections with I 〉 2δ(I). The crystal of compound 2 is of monoclinic system, space group P21/n, with a = 13.050(4), b = 20.577(5), c = 13.323(4)A,β = 113.578(3)°, V = 3227.2(14)A3, Z = 2, C64H48F12Mn2N10O8P2, Mr = 1484.94, Dc = 1.528 g/cm^3, F(000) = 1508.0, Rint= 0.0295, T= 293(2) K,μ = 0.539 mm^-1, the final R = 0.0629 and wR = 0.1789 for 5298 observed reflections with I 〉 2σ(I). Compounds 1 and 2 are linear trinuclear and dinuclear manganese complexes respectively, which are both bridged by carboxylate groups of the ligands.
基金The project was supported by the Education Department of Zhejiang Province (20030710)
文摘The title complex, C18H15N3NiO3, has been prepared and characterized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group Cc with a = 10.939(2), b = 22.909(5), c = 6.907(1) ?, β = 116.75(3)°, V = 1545.7(5) ?, Z = 4, Mr = 380.04, F(000) = 784, Dc = 1.633 g/cm3 and μ(MoKα) = 1.279 mm–1. The structure was refined to R = 0.0472 and wR = 0.0893 for 2571 observed reflections with I > 2σ(I). The absolute structure Flack parameter X is 0.01(2). In this crystal structure, strong face-to-face π-π stacking interactions between adjacent molecules lead to a one-dimensional chain structure.
文摘The comparative process for preparing 9-oxime erythromycin A (EMAO) is investigated. EMAO was synthesized and compared by the reaction of erythromycin and hydroxylamine hydrochloride with various bases such as sodium acetate, triethylamine, etc. A new synthetic method is established. The oximation is performed under dynamic buffer system; less degradation impurities are formed. The yield of EMAO reaches more than 95%, HPLC analysis shows that the purity of EMAO is more than 90%, and the E/Z isomeric ratio preponderates over 7∶1.
文摘The Beckmann rearrangement of cyclohexanone oxime was achieved by the combined use of cobalt salt and Lewis acids co-catalysts (each 10 mol%). Various combinations of cobalt salts and Lewis acids gave lactams in a satisfactory yield under mild conditions. This method makes it possible to reduce undesirable byproducts.
文摘A series of novel flavone-4-oximes[1]were synthesized by the oximation of substituted flavones.The synthesized compounds were characterized by various spectroscopic methods including IR,MASS,NMR spectroscopy.Out of the 14 test compounds screened for their antioxidant activity,compounds such as JGS-VI(a N,N dimethyl benzaldehyde derivative)and JGSVII(a 3,4 dimethoxy benzaldehyde derivative)exhibited antioxidant activity comparable to that of ascorbic acid with its IC50 value at 30.01 Mm as standard following DPPH?method.Compounds such as JGS-II(a Para fluro benzaldehyde derivative),JGS-IV(a Para methyl benzaldehyde derivative)and JGS-V(a thiophene-2-aldehyde derivative)exhibited anti-oxidant activity among all the test compounds screened against ABTS[2]using Quercetin with its IC50 value at 50.24 Mm.
基金Afyon Kocatepe Universty Research Fund(No.06-FENED-09)
文摘The synthesis of two new methacrylates such as 2-[(cyclohexylideneamino)oxy]-2-oxoethyl methylacrylate (CHOEMA)and 2-[(cyclopentylideneamino)oxy]-2-oxoethyl methylacrylate(CPOEMA)are described.The monomers produced from the reaction of corresponding cyclohexanone O-(2-chloroacetyl)oxime and cyclopentanone O-(2- chloroacetyl)oxime with sodium methacrylate was polymerized in 1,4-dioxane solution at 65℃using AIBN as an initiator. The monomers and their polymers were characterized by IR,~1H- and ^(13)C-NMR spec...
文摘The addition of platinum over the B2O3/TiO2-ZrO2 remarkably enhanced its catalytic stability in the vapor phase Beckmann rearrangement of cyclohexanone oxime under the carder gas of H2. The content of coke deposited on catalyst surface was decreased from 1.92% over the B2O3/TiO2-ZrO2 to 1.14% over the platinum promoted B2O3/TiO2-ZrO2 after reaction of six hours. This result indicates that the platinum added on the B2O3/TiO2-ZrO2 catalyst plays an important role in reducing the coke formation on the catalyst surface.
基金Supported by Natural Science Fund of Heilongjiang Province(C201424)
文摘The pharmacokinetics of milbemycin oxime was investigated in dogs following oral(per os, PO) and intravenous(IV) administration. Three groups of dogs received milbemycin oxime tablets as a single PO dose equal to 0.25, 0.5 and 1.0 mg · kg-1 of milbemycin oxime, respectively, another group received a single IV dose of 0.5 mg · kg-1. Blood samples were collected at predetermined times after drug administration and the milbemycin oxime concentrations in plasma were determined by LC-MS/MS. The drug protein binding in dog plasma in vitro was determined by equilibrium dialysis at concentrations spanning the range of values observed in vivo in dog plasma. After PO administration at doses of 0.25, 0.5 and 1.0 mg · kg-1, milbemycin oxime was slowly absorbed and eliminated, the time to reach the maximum plasma concentration(Tmax) was 4.14±0.20, 4.27±0.14 and 4.06±0.13 h, the mean absorption time(MAT) was 19.06, 13.67 and 11.77 h, the terminal rate half-life(t1/2λz) was 15.06±0.37, 11.09±0.54 and 9.76±0.89 h and the total body clearance(Cl) was 1.15±0.05, 1.18±0.03 and 1.17±0.07 m L · min-1 · kg-1, respectively. The maximum plasma concentration(Cmax, 36.50±1.40, 76.11±2.77 and 182.05±7.20 ng · m L-1, respectively) and the area under the first-moment curve(AUC-10→∞, 985.83±49.46, 1 663.12±51.42 and 3 558.04±197.88 mg · h · L, respectively) increased accordingly to the administered dose rates; the oral bioavailabilities were estimated to be 88.61%, 74.75% and 79.96%, respectively. The values of fu were 0.12%, 0.14% and 0.13% in dog plasma, respectively. In conclusion, the pharmacokinetics of milbemycin oxime in dogs following oral administration revealed its higher oral bioavailability and advantageous pharmacokinetic properties, such as its lower total body clearance and longer elimination half-life, and indicated that the single oral dose of 0.50 mg · kg-1 of milbemycin oxime which was recommended in all the parasitological efficacy studies allowed an adequate concentration of the drug.
基金The project was supported by the National Natural Science Foundation of China(No 20272018)the Guangdong Natural Science Foundation(No 021166,04010458)the Scientific Research Foundation for the Retumed Overseas Chinese Scholars,State Education Ministry of China.
基金The project was supported by the Natural Science Foundation of Shandong Province (No. Z2004C06)National Basic Research Priority Program (2003CCA027)
文摘A novel derivative of glycyrrhetinic acid, (E)-ethyl 3-keto-18β-glycyrrhetinate 3- oxime C32H49NO4 (Mr = 511.72), was synthesized and structurally characterized by IR, 1^H NMR and single-crystal X-ray diffraction. It belongs to monoclinic, space group P21, with a = 12.4897(12), b = 7.3190(7), c = 15.9944(14)A, β = 94.833(2)o, V = 1456.9(2)A^3, Z = 2, Dc = 1.167 g/cm^3, μ = 0.075 mm^-1, F(000) = 560, the final R = 0.0449 and wR = 0.1122. A total of 7486 reflections were collected, of which 2785 were independent (Rint = 0.0199) and 2605 were observed with I 〉 2σ(I). There exists an intermolecular hydrogen bond which helps to stabilize the crystal structure.
基金the Student Research Train Project of Anhui University of Technology(No.08021)
文摘Eleven new 1-{5-[4-(benzyloxy)phenyl]-3-methyl-4,5-dihydropyrazol-l-yl} oxime ester dcrivatives were synthesized and characterized by elemental analysis, HRMS, ^1H NMR data. All the compounds were screened for their antibacterial potential in vitro against Bacillus subtilis, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa. The results indicate that compounds 8c and 8f possess potent activity with the minimum inhibitory concentrations(MIC) of 1.562--3.125 ug/mL against all the four bacteria. Compounds 8c, 8e and 8f show moderate inhibition against the DNA gyrase(IC50=1.9--2.5 ug/mL). On the basis of the biological activities, structure-activity relationship was discussed.