为了改善天然黄酮的药理活性,本文将苯环三甲氧基引入黄酮骨架,对5,6,7-三甲氧基黄酮类化合物的合成路线进行了改进。以3,4,5-三甲氧基苯酚为原料,通过Friedel-Crafts反应生成氯苯乙酮,再与对羟基苯甲醛环合得到4-羟基-5,6,7-三甲氧基...为了改善天然黄酮的药理活性,本文将苯环三甲氧基引入黄酮骨架,对5,6,7-三甲氧基黄酮类化合物的合成路线进行了改进。以3,4,5-三甲氧基苯酚为原料,通过Friedel-Crafts反应生成氯苯乙酮,再与对羟基苯甲醛环合得到4-羟基-5,6,7-三甲氧基黄酮。其结构经1H NMR,13 C NMR及MS(ESI)表征,总产率为61%。与传统黄酮合成路线对比,该方案简化了合成路线、提高了反应产率、解决了实验后处理难等问题,是一种适合黄酮工业化生产的合成方法。展开更多
A field experiment was employed to study the degradation of triadimefon and difenoconazole residues in strawberry and soil. The results showed that the degradation of both the two kinds of pesticides was in accordance...A field experiment was employed to study the degradation of triadimefon and difenoconazole residues in strawberry and soil. The results showed that the degradation of both the two kinds of pesticides was in accordance with the first order kinetic equation. The half-lives of difenoconazole in strawberry fruit, strawberry stem leaf and soil were 4.09, 8.21 and 13.38 d, respectively; and the half-lives of triadimefon in strawberry fruit, strawberry stem and leaf and soil were 3.38, 5.31 and 15.64 d, respectively. The maximum residue limit （MRL） of difenoconazole in strawberry was recommended as 0.5 mg/kg, and 10% difenoconazole WG and 20% triadimefon EC should be applied four times with a safety interval of 7 d according to the amounts of 100 and 60 g a. i./hm2,respectively.展开更多
AIM： To explore the possible mechanisms of curcumin in rat colitis induced by trinitrobenzene sulfonic （TNBS） acid. METHODS： Rats with TNBS acid-induced colitis were treated with curcumin （30 mg/kg or 60 mg/kg pe...AIM： To explore the possible mechanisms of curcumin in rat colitis induced by trinitrobenzene sulfonic （TNBS） acid. METHODS： Rats with TNBS acid-induced colitis were treated with curcumin （30 mg/kg or 60 mg/kg per day ip）. Changes of body weight and histological scores as well as survival rate were evaluated. Leukocyte infiltration was detected by myeloperoxidase （MPO） activity assay. The expression of cyclooxygenase-2 （COX-2） was detected by RT-PCR and Western blot. Inflammation cytokines were determined by RT-PCR. Local concentration of prostaglandin E2 （PGE2） in colon mucosa was determined by ELISA. RESULTS： Curcumin improved survival rate and histological image, decreased the macroscopic scores and MPO activity. Also curcumin reduced the expression of COX-2 and inflammation cytokines. In addition, treatment with curcumin increased the PGE2 level. CONCLUSION： Curcumin has therapeutic effects on TNBS acid-induced colitis, the mechanisms seem to be related to COX-2 inhibition and PGE2 improvement.展开更多
The title compound 〔(PPh 3)(CH 3COS) 2NiB 10 H 10 〕·0.4(C 5H 12 ) has been synthesized by the reaction of 〔NiCl 2(PPh 3) 2〕, closo 〔B 10 H 10 〕 2- and CH 3COSH in CH 2Cl 2 solution. It was recrystallized fr...The title compound 〔(PPh 3)(CH 3COS) 2NiB 10 H 10 〕·0.4(C 5H 12 ) has been synthesized by the reaction of 〔NiCl 2(PPh 3) 2〕, closo 〔B 10 H 10 〕 2- and CH 3COSH in CH 2Cl 2 solution. It was recrystallized from n pentane/CH 2Cl 2 solution and its structure was determined by X ray diffraction analysis. The crystal is triclinic, space group P1, M r= 618.23, with a=10.049(1), b=12.638(2), c=14.077(2) , α=110.13(1), β=87.65(1), γ=96.01(1)°, V=1669.3(4) 3, D c =1.230 g/cm 3, Z=2, λ (Mo Kα )=0.71073 , μ =7.76 cm -1 , F (000)=642. The final refinement is converged with R =0.042 (5986 observed reflections with I≥2σ(I)), wR 2 =0.151. The cluster is a nido eleven vertex {NiB 10 } cage with the Ni atom in the open NiB 4 face. Cyclizations resulting in two five membered rings, Ni(7)-S(1)-C(1)-O(1)-B(2) and Ni(7)-S(2)-C(2)-O(2)-B(3), have occurred.展开更多
Rhodium-catalyzed cycloaddition reaction was calculated by density functional theory M06-2X method to directly synthesize benzoxepine and coumarin derivatives.In this work,we conducted a computational study of two com...Rhodium-catalyzed cycloaddition reaction was calculated by density functional theory M06-2X method to directly synthesize benzoxepine and coumarin derivatives.In this work,we conducted a computational study of two competitive mechanisms in which the carbon atom of acetylene or carbon monoxide attacked and inserted from two different directions of the six-membered ring reactant to clarify the principle characteristics of this transformation.The calculation results reveal that:(i)the insertion process of alkyne or carbon monoxide is the key step of the reaction;(ii)for the(5+2)cycloaddition reaction of acetylene,higher energy is required to break the Rh−O bond of the reactant,and the reaction tends to complete the insertion from the side of the Rh−C bond;(iii)for the(5+1)cycloaddition of carbon monoxide,both reaction paths have lower activation free energy,and the two will generate a competition mechanism.展开更多
An ion-pair compound, [HL]2[Ni(CN)4]4H2O 1 has been obtained as an unexpected product when we attempt to prepare a heterometallic cyano-bridged complex by the reaction of GdCl3nH2O, K2Ni(CN)4 and L (L=4-(2-hydroxyphen...An ion-pair compound, [HL]2[Ni(CN)4]4H2O 1 has been obtained as an unexpected product when we attempt to prepare a heterometallic cyano-bridged complex by the reaction of GdCl3nH2O, K2Ni(CN)4 and L (L=4-(2-hydroxyphenyl)-1,5,9-triazacyclododecan-2-one) in aqueous solution, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.380(1), b = 9.9637(8), c = 17.087(1) ? ?= 105.947(2)? V = 2026.6(3) ?, Rint = 0.0509, Z = 2, Dc = 1.297 g/cm3, C34H56O8N10Ni, Mr = 791.60, F(000) = 844, m(MoKa) = 0.538 mm1, S = 1.030, the final R = 0.0644 and wR = 0.1299 for 2023 observed reflections with I ≥ 2(I). The title compound 1 contains one anion of [Ni(CN)4]2, two cations of [HL]+ and four packing water molecules, which are held together by the NH···O and OH···O hydrogen bonds to form a three- dimensional framework.展开更多
The aim of the current work is to create new heterocyclic tetracyclic condensed systems which combine benzothiofen and benzimidazoleinto one molecule. The haisic products are 1,2-, 2,3- and 3,4- diamines of dibenzothi...The aim of the current work is to create new heterocyclic tetracyclic condensed systems which combine benzothiofen and benzimidazoleinto one molecule. The haisic products are 1,2-, 2,3- and 3,4- diamines of dibenzothiophenes. Orto-diamines react with hydrochloric acid and sodium nitrite and obtain three new isomeric heterocyclic systems： 3H-benzothieno[3,2-e]benzotriazole, 3H-benzothieno[2,3-f]benzotriazole and 1H-benzothieno[3,2-g]benzotriazole with the anticipated biological activity. Their spectral characteristics are studied.展开更多
The title compound, 1,12,15 triaza 3,4:9,10 dibenzo 5,8 dioxacyclopentadecane N acetic lactam (C 22 H 29 N 3O 3Br 2, M r =543.29) has been synthesized and characterized by analytical data, IR and 1HNMR spectra. The co...The title compound, 1,12,15 triaza 3,4:9,10 dibenzo 5,8 dioxacyclopentadecane N acetic lactam (C 22 H 29 N 3O 3Br 2, M r =543.29) has been synthesized and characterized by analytical data, IR and 1HNMR spectra. The compound crystallizes in the trigonal system, space group R 3 with a = 35.194(1), c = 10.397(1) , γ=120°, V=11152.6(1) 3, Z=18, D c =1.456 gcm -3 , F(000)=4968, μ =3.3 mm -1 . Mo Kα radiation ( λ = 0.71073), R = 0.0145 for 3094 observed reflections 〔 I>2σ(I )〕 of 3392 independent reflections. The result shows that monofunction reaction for polyaza macrocycle were protonized. 1H NMR spectra of the ligand showed two sets of multiplets due to the two phenyl rings of the ligand in different environments.展开更多
The crystal and molecular structure of 4, 5-trans-2-amino-1, 3, 3-tri-cyano-4, 5-di(4-chlorophenyl) cyclopentene. ethanol - monohydrate has been deter-mined by X-ray diffraction method. The crystal (C20H12N4Cl2. C2H6O...The crystal and molecular structure of 4, 5-trans-2-amino-1, 3, 3-tri-cyano-4, 5-di(4-chlorophenyl) cyclopentene. ethanol - monohydrate has been deter-mined by X-ray diffraction method. The crystal (C20H12N4Cl2. C2H6O. H2O, Mr=443. 33) is triclinic with space group P1, a= 11. 033(4), b= 12. 199(3), c= 10. 732(3) A, a=114. 46(2), β=118. 33(3) γ=81. 56(3), V=1155- 1(7) A3, Z=2, Dc= 1. 275g/cm3, μ(MoKa) = 3. 05cm-1, F(000) = 460, R= 0. 070, Rw = 0. 089 for1965 observed reflections (I>3(I)). The phenyl groups are in equatorial positionsand form dihedral angles of 67. 89 and 63. 77° with the central 5-ring. X-ray analysisreveals that in the five membered ring the C (1) -C (2) bond is longer than normal double C=C bond while the C(2) -N (2) bond is shorter than normal C(sp)2-N bond.展开更多
文摘为了改善天然黄酮的药理活性,本文将苯环三甲氧基引入黄酮骨架,对5,6,7-三甲氧基黄酮类化合物的合成路线进行了改进。以3,4,5-三甲氧基苯酚为原料,通过Friedel-Crafts反应生成氯苯乙酮,再与对羟基苯甲醛环合得到4-羟基-5,6,7-三甲氧基黄酮。其结构经1H NMR,13 C NMR及MS(ESI)表征,总产率为61%。与传统黄酮合成路线对比,该方案简化了合成路线、提高了反应产率、解决了实验后处理难等问题,是一种适合黄酮工业化生产的合成方法。
基金Supported by Tripartite Joint Fund of Science and Technology Department of Guizhou Province(LH[2016]7278)Agricultural Science and Technology Project of Science and Technology Department of Guizhou Province(NZ[2013]3029)+1 种基金Tripartite Joint Fund of Science and Technology Department of Guizhou Province(Key Project)(JLKA[2012]03)Natural Science Research Project of Department of Education of Guizhou Province(2011054)~~
文摘A field experiment was employed to study the degradation of triadimefon and difenoconazole residues in strawberry and soil. The results showed that the degradation of both the two kinds of pesticides was in accordance with the first order kinetic equation. The half-lives of difenoconazole in strawberry fruit, strawberry stem leaf and soil were 4.09, 8.21 and 13.38 d, respectively; and the half-lives of triadimefon in strawberry fruit, strawberry stem and leaf and soil were 3.38, 5.31 and 15.64 d, respectively. The maximum residue limit （MRL） of difenoconazole in strawberry was recommended as 0.5 mg/kg, and 10% difenoconazole WG and 20% triadimefon EC should be applied four times with a safety interval of 7 d according to the amounts of 100 and 60 g a. i./hm2,respectively.
文摘AIM： To explore the possible mechanisms of curcumin in rat colitis induced by trinitrobenzene sulfonic （TNBS） acid. METHODS： Rats with TNBS acid-induced colitis were treated with curcumin （30 mg/kg or 60 mg/kg per day ip）. Changes of body weight and histological scores as well as survival rate were evaluated. Leukocyte infiltration was detected by myeloperoxidase （MPO） activity assay. The expression of cyclooxygenase-2 （COX-2） was detected by RT-PCR and Western blot. Inflammation cytokines were determined by RT-PCR. Local concentration of prostaglandin E2 （PGE2） in colon mucosa was determined by ELISA. RESULTS： Curcumin improved survival rate and histological image, decreased the macroscopic scores and MPO activity. Also curcumin reduced the expression of COX-2 and inflammation cytokines. In addition, treatment with curcumin increased the PGE2 level. CONCLUSION： Curcumin has therapeutic effects on TNBS acid-induced colitis, the mechanisms seem to be related to COX-2 inhibition and PGE2 improvement.
文摘The title compound 〔(PPh 3)(CH 3COS) 2NiB 10 H 10 〕·0.4(C 5H 12 ) has been synthesized by the reaction of 〔NiCl 2(PPh 3) 2〕, closo 〔B 10 H 10 〕 2- and CH 3COSH in CH 2Cl 2 solution. It was recrystallized from n pentane/CH 2Cl 2 solution and its structure was determined by X ray diffraction analysis. The crystal is triclinic, space group P1, M r= 618.23, with a=10.049(1), b=12.638(2), c=14.077(2) , α=110.13(1), β=87.65(1), γ=96.01(1)°, V=1669.3(4) 3, D c =1.230 g/cm 3, Z=2, λ (Mo Kα )=0.71073 , μ =7.76 cm -1 , F (000)=642. The final refinement is converged with R =0.042 (5986 observed reflections with I≥2σ(I)), wR 2 =0.151. The cluster is a nido eleven vertex {NiB 10 } cage with the Ni atom in the open NiB 4 face. Cyclizations resulting in two five membered rings, Ni(7)-S(1)-C(1)-O(1)-B(2) and Ni(7)-S(2)-C(2)-O(2)-B(3), have occurred.
基金This work was supported by the Natural Science Foundation of Gansu Province(20JR5RA479)the Outstanding Youth Research Program of Lanzhou University of Arts and Sciences(2018JCQN008).
文摘Rhodium-catalyzed cycloaddition reaction was calculated by density functional theory M06-2X method to directly synthesize benzoxepine and coumarin derivatives.In this work,we conducted a computational study of two competitive mechanisms in which the carbon atom of acetylene or carbon monoxide attacked and inserted from two different directions of the six-membered ring reactant to clarify the principle characteristics of this transformation.The calculation results reveal that:(i)the insertion process of alkyne or carbon monoxide is the key step of the reaction;(ii)for the(5+2)cycloaddition reaction of acetylene,higher energy is required to break the Rh−O bond of the reactant,and the reaction tends to complete the insertion from the side of the Rh−C bond;(iii)for the(5+1)cycloaddition of carbon monoxide,both reaction paths have lower activation free energy,and the two will generate a competition mechanism.
文摘An ion-pair compound, [HL]2[Ni(CN)4]4H2O 1 has been obtained as an unexpected product when we attempt to prepare a heterometallic cyano-bridged complex by the reaction of GdCl3nH2O, K2Ni(CN)4 and L (L=4-(2-hydroxyphenyl)-1,5,9-triazacyclododecan-2-one) in aqueous solution, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.380(1), b = 9.9637(8), c = 17.087(1) ? ?= 105.947(2)? V = 2026.6(3) ?, Rint = 0.0509, Z = 2, Dc = 1.297 g/cm3, C34H56O8N10Ni, Mr = 791.60, F(000) = 844, m(MoKa) = 0.538 mm1, S = 1.030, the final R = 0.0644 and wR = 0.1299 for 2023 observed reflections with I ≥ 2(I). The title compound 1 contains one anion of [Ni(CN)4]2, two cations of [HL]+ and four packing water molecules, which are held together by the NH···O and OH···O hydrogen bonds to form a three- dimensional framework.
文摘The aim of the current work is to create new heterocyclic tetracyclic condensed systems which combine benzothiofen and benzimidazoleinto one molecule. The haisic products are 1,2-, 2,3- and 3,4- diamines of dibenzothiophenes. Orto-diamines react with hydrochloric acid and sodium nitrite and obtain three new isomeric heterocyclic systems： 3H-benzothieno[3,2-e]benzotriazole, 3H-benzothieno[2,3-f]benzotriazole and 1H-benzothieno[3,2-g]benzotriazole with the anticipated biological activity. Their spectral characteristics are studied.
文摘The title compound, 1,12,15 triaza 3,4:9,10 dibenzo 5,8 dioxacyclopentadecane N acetic lactam (C 22 H 29 N 3O 3Br 2, M r =543.29) has been synthesized and characterized by analytical data, IR and 1HNMR spectra. The compound crystallizes in the trigonal system, space group R 3 with a = 35.194(1), c = 10.397(1) , γ=120°, V=11152.6(1) 3, Z=18, D c =1.456 gcm -3 , F(000)=4968, μ =3.3 mm -1 . Mo Kα radiation ( λ = 0.71073), R = 0.0145 for 3094 observed reflections 〔 I>2σ(I )〕 of 3392 independent reflections. The result shows that monofunction reaction for polyaza macrocycle were protonized. 1H NMR spectra of the ligand showed two sets of multiplets due to the two phenyl rings of the ligand in different environments.
文摘The crystal and molecular structure of 4, 5-trans-2-amino-1, 3, 3-tri-cyano-4, 5-di(4-chlorophenyl) cyclopentene. ethanol - monohydrate has been deter-mined by X-ray diffraction method. The crystal (C20H12N4Cl2. C2H6O. H2O, Mr=443. 33) is triclinic with space group P1, a= 11. 033(4), b= 12. 199(3), c= 10. 732(3) A, a=114. 46(2), β=118. 33(3) γ=81. 56(3), V=1155- 1(7) A3, Z=2, Dc= 1. 275g/cm3, μ(MoKa) = 3. 05cm-1, F(000) = 460, R= 0. 070, Rw = 0. 089 for1965 observed reflections (I>3(I)). The phenyl groups are in equatorial positionsand form dihedral angles of 67. 89 and 63. 77° with the central 5-ring. X-ray analysisreveals that in the five membered ring the C (1) -C (2) bond is longer than normal double C=C bond while the C(2) -N (2) bond is shorter than normal C(sp)2-N bond.
