以N,N-二甲基甲酰胺作溶剂,2-对甲苯乙炔基苯酚和α-环己烯酮在氯化钯和四丁基碘化铵的作用下,可以顺利发生分子内环化反应一步合成3-(2-对甲苯基苯并呋喃-3-基)环己-2-烯酮。反应最佳条件为:n(2-对甲苯乙炔基苯酚)∶n(α-环己烯酮)∶n...以N,N-二甲基甲酰胺作溶剂,2-对甲苯乙炔基苯酚和α-环己烯酮在氯化钯和四丁基碘化铵的作用下,可以顺利发生分子内环化反应一步合成3-(2-对甲苯基苯并呋喃-3-基)环己-2-烯酮。反应最佳条件为:n(2-对甲苯乙炔基苯酚)∶n(α-环己烯酮)∶n(氯化钯)∶n(四丁基碘化铵)=1∶5∶0.05∶1,反应温度为100℃,反应时间为24h,反应最佳产率82.0%。产物经1 H NMR、13 CNMR和GC-MS确征。展开更多
Green oxidation of cyclohexene using dioxygen as oxidizing agent is highly desirable because of its environmental compatibility and economic impact. Separation of its oxidation products depends on the reliable vaporli...Green oxidation of cyclohexene using dioxygen as oxidizing agent is highly desirable because of its environmental compatibility and economic impact. Separation of its oxidation products depends on the reliable vaporliquid equilibrium （VLE） data of relevant components, which are still lacking. The VLE data of binary system 1,2-epoxycyclohexane and 2-cyclohexen-l-one under ambient pressure were obtained using an improved VLE equipment EC-2 still in this work. The results showed that this binary system has no azeotropic point. Furthermore, the experimental VLE data were correlated with the Wilson thermodynamic model and the corresponding binary interaction parameters of the model were obtained. The results showed that the VLE data agreed well with the model and passed the thermodynamic consistency test of Herrington.展开更多
Hydroxy-phenyl)-5-(2-methyl-phenyl)-6-ethoxycarbonyl-cyclohexen-2-one has been synthesized and characterized by elemental analysis, IR, UV, H NMR and MS, and its crystal 1 structure was determined by X-ray single-crys...Hydroxy-phenyl)-5-(2-methyl-phenyl)-6-ethoxycarbonyl-cyclohexen-2-one has been synthesized and characterized by elemental analysis, IR, UV, H NMR and MS, and its crystal 1 structure was determined by X-ray single-crystal diffraction method. The crystal belongs to the monoclinic system, space group P21/c with a = 14.6298(13), b = 5.8623(5), c = 22.255(2) ?, β = 105.855(2)o, V = 1836.0(3) ?3, Mr = 350.40, Z = 4, Dc = 1.268 g/cm3, F(000) = 744, μ(MoKα) = 0.086 mm-1, R = 0.0680 and wR = 0.1498. The crystal analysis results show that the cyclohexene unit of the title compound has a quasi-chair conformation, and a centrosymmetric dimer with a 16-membered ring is produced by the intermolecular hydrogen bonds.展开更多
The title compound 4, 5-bis ( 2,-dinitrophenylthio )-1, 3-dithiole-2-thione [C3S5(C6H3N2O4)2] crystallizes in the orthogonal system, space group P212121,with a=10. 134(3) , b=20. 488(4), c=9. 656(3)A , V=2005. 1 A3, D...The title compound 4, 5-bis ( 2,-dinitrophenylthio )-1, 3-dithiole-2-thione [C3S5(C6H3N2O4)2] crystallizes in the orthogonal system, space group P212121,with a=10. 134(3) , b=20. 488(4), c=9. 656(3)A , V=2005. 1 A3, D_c=1. 76 g/cm￣3 , Z=4, M.=530. 56, λ=0. 71069 A, F(000)= 1072 , μ=6.1 cm￣(-1), T=296K.Final R= 0. 038, R.= 0. 045 for 1799 reflections with I≥3.5σ(I). In this nonplanar neutral molecule both nitrobenzol rings are approximately perpendicular to the dithiole ring with an asymmetric configuration.展开更多
The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characteriz...The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characterized by X ray diffraction study, IR and UV Vis spectroscopy. Crystallographic data : space group: P2 1/n, a=11.843(2), b=11 079(1), c = 15.404(1) , β=110.33(1)°, V = 1895.1 3, Z=2, D c =1.62 g/cm 3 , μ =17.6 cm -1 , F (000)=956, R=0.052, R w =0.061. In the structure of the title complex, the tto (tto=tetrathioxalato) ligand in bridging form is chelated to two nickel atoms and dmit (dmit=1,3 dithiole 2 thione 4,5 dithiolate) ligands coordinated to nickel atoms.展开更多
文摘以N,N-二甲基甲酰胺作溶剂,2-对甲苯乙炔基苯酚和α-环己烯酮在氯化钯和四丁基碘化铵的作用下,可以顺利发生分子内环化反应一步合成3-(2-对甲苯基苯并呋喃-3-基)环己-2-烯酮。反应最佳条件为:n(2-对甲苯乙炔基苯酚)∶n(α-环己烯酮)∶n(氯化钯)∶n(四丁基碘化铵)=1∶5∶0.05∶1,反应温度为100℃,反应时间为24h,反应最佳产率82.0%。产物经1 H NMR、13 CNMR和GC-MS确征。
基金Supported by Outstanding Personality Innovation Funds of Henan Province (0121001900)
文摘Green oxidation of cyclohexene using dioxygen as oxidizing agent is highly desirable because of its environmental compatibility and economic impact. Separation of its oxidation products depends on the reliable vaporliquid equilibrium （VLE） data of relevant components, which are still lacking. The VLE data of binary system 1,2-epoxycyclohexane and 2-cyclohexen-l-one under ambient pressure were obtained using an improved VLE equipment EC-2 still in this work. The results showed that this binary system has no azeotropic point. Furthermore, the experimental VLE data were correlated with the Wilson thermodynamic model and the corresponding binary interaction parameters of the model were obtained. The results showed that the VLE data agreed well with the model and passed the thermodynamic consistency test of Herrington.
基金This work was financially supported by the Education Committee of Hunan Province (02C465)Hunan Provincial Key Discipline and Hunan Provincial General College Leader of Learning
文摘Hydroxy-phenyl)-5-(2-methyl-phenyl)-6-ethoxycarbonyl-cyclohexen-2-one has been synthesized and characterized by elemental analysis, IR, UV, H NMR and MS, and its crystal 1 structure was determined by X-ray single-crystal diffraction method. The crystal belongs to the monoclinic system, space group P21/c with a = 14.6298(13), b = 5.8623(5), c = 22.255(2) ?, β = 105.855(2)o, V = 1836.0(3) ?3, Mr = 350.40, Z = 4, Dc = 1.268 g/cm3, F(000) = 744, μ(MoKα) = 0.086 mm-1, R = 0.0680 and wR = 0.1498. The crystal analysis results show that the cyclohexene unit of the title compound has a quasi-chair conformation, and a centrosymmetric dimer with a 16-membered ring is produced by the intermolecular hydrogen bonds.
文摘The title compound 4, 5-bis ( 2,-dinitrophenylthio )-1, 3-dithiole-2-thione [C3S5(C6H3N2O4)2] crystallizes in the orthogonal system, space group P212121,with a=10. 134(3) , b=20. 488(4), c=9. 656(3)A , V=2005. 1 A3, D_c=1. 76 g/cm￣3 , Z=4, M.=530. 56, λ=0. 71069 A, F(000)= 1072 , μ=6.1 cm￣(-1), T=296K.Final R= 0. 038, R.= 0. 045 for 1799 reflections with I≥3.5σ(I). In this nonplanar neutral molecule both nitrobenzol rings are approximately perpendicular to the dithiole ring with an asymmetric configuration.
文摘The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characterized by X ray diffraction study, IR and UV Vis spectroscopy. Crystallographic data : space group: P2 1/n, a=11.843(2), b=11 079(1), c = 15.404(1) , β=110.33(1)°, V = 1895.1 3, Z=2, D c =1.62 g/cm 3 , μ =17.6 cm -1 , F (000)=956, R=0.052, R w =0.061. In the structure of the title complex, the tto (tto=tetrathioxalato) ligand in bridging form is chelated to two nickel atoms and dmit (dmit=1,3 dithiole 2 thione 4,5 dithiolate) ligands coordinated to nickel atoms.
