简介:利用L-脯氨酸催化的5-氯水杨醛(1)与6-甲基-4-羟基吡喃酮(2)的缩合反应及硫酸铜催化下与1,3-二甲基-5-氨基吡唑(3)的串联反应,合成得到了10-氯-1,3-二甲基-5-(2-氧代丙基)色烯并[4,3-d]吡唑并[3,4-b]吡啶-6(3H)-酮(4)和10-氯-5-二乙氧基甲基-1,3-二甲基色烯并[4,3-d]吡唑并[3,4-b]吡啶-6(3H)-酮(5).化合物5的结构通过单晶X射线衍射法确定:晶体属于三斜晶系,空间群P-1;相对分子质量Mr=803.68;晶胞参数a=1.03160(10)nm,b=1.42900(13)nm,c=1.44268(15)nm;V=1.9448(3)nm~3;Z=2;晶胞密度Dc=1.372g/cm~3;吸收系数μ=0.228mm-1;单胞中电子的数目F(000)=840.晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R=0.0681,wR=0.2051.在晶体结构中色烯环与吡啶环及吡唑环近似于共平面.
简介:Sixnewopticallyactivepoly(amide-imide)s(5a-f)weresynthesizedthroughthedirectpolycondensationreactionofN,N'-(4,4'-diphthaloyl)-bis-L-leucine(3)withsixhydantoinderivatives(4a-f).Triphenylphosphite(TPP)/pyridineinthepresenceofcalciumchloride(CaCl_2)andN-methyl-2-pyrrolidone(NMP)weresuccessfullyappliedfordirectpolycondensation.Thepolycondensationreactionsproduceaseriesofnewpoly(amide-imide)s(5a-f)inhighyields,andinherentviscositybetween0.42and0.55dL/g.Theresultingpoly(amide-imide)s(5a-f)werecharacterizedbyelementalanalysis,viscositymeasurements,thermalgravimetricanalysis(TGAandDTG),solubilitytestandFT-IRspectroscopy.
简介:AseriesofmesoporousCu-Mn-Al2O3(CMA)materialswassynthesizedatmoderatetemperatureandtheirstructureswerecharacterizedbyXRD,N2physicaladsorptionandTPRtechniques.Itwasfoundthatusingmetalcomplexion[Cu(NH3)42+-Mn(NH3)62+]asrawmaterialsiseasiertoformgood-structuremesoporousCu-Mn-Al2O3materialsthanusingitsnitratesalt[Cu(NO3)2-Mn(NO3)2].TheTPRtestsresultsindicatethatCuOandMnOxwerehomogeneouslydispersedinthemesoporousmaterials.TheircatalyticapplicationtopreferentialcatalyticoxidationofCOinahydrogen-richstreamwasstudied.TheactivityvariesintheorderofCMA(1:1,molarratio)>CMA(1:2)>CMA(2:1)>CMA(CP)>CMA(1:0)≈CMA(0:1).TheCMA(1:0)andCMA(0:1)haveloweractivitycomparedtoothersamples,implyingthatthereexistedcoordinationeffectbetweenCu-Mninthesamples.TheselectivityvariedintheorderofCMA(0:1)≥CMA(1:2)>CMA(1:1)>CMA(2:1)>CMA(1:0)athighertemperature(≥120°C),indicatingthatincreasingtheCucontentenhancedtheconversionofH2.ThesampleCMA(CP)madebycoprecipitationmethodhasalowerCOoxidationactivityandselectivitythanitscounter-partsofmesoporousCu-Mn-Al2O3materials[CMA(1:2)],thisattributedtothelowersurfaceareaoftheformerandpoorinteractionofCuOwithMnOx.
简介:利用电介质的平均能带模型计算了PrBa2Cu3O7的化学键参数,得到Cu(1)-O键的人价性为0.41,Cu(2)-O键的平均共价性为0.28,应用由共价性和要化率定义的化学环境因子计算了^57Fe在PrBa2Cu3O7中的Mossbauer同质异能位移,确定了^57Fe在PrBa2Cu3O7中的价态和占位情况。
简介:Wehavesuccessfullysynthesized1-(2′-Phenyl)cycloproply1-2,3-epoxypropan-1-ol3,whichwillbeappliedtothekineticsstudyofoxiranylcarbinylradical.
简介:Anovelseriesofpyrido[1,2-e]purin-4(3H)-onederivativescontainingpolarsubstituentson5'-positionweredesignedandpreparedaspotentialPDE5inhibitors.Thispaperreportsthesyntheticroutes,1H-NMRdata,andthePDE5inhibitoryactivitiesofthetargetcompounds.Thepolarpiperazinylgroupcontained(on5'-position)compound,3B2,showedthehighestactivityamongthetestedderivativesbutlesspotencythansildenafil1.
简介:采用水热方法合成一种新型钼-氧簇化合物Ni(en)3MoO4,并通过X射线单晶结构分析、红外光谱分析、元素分析、差热热重分析对该化合物进行了表征.结构分析数据表明:该化合物属三方晶系,P-31c空间群,晶胞参数a=0.9226(13)nm,b=0.9226(13)nm,c=0.9959(2)cm,α=90°,β=90°,γ=120°,V=0.7342(2)nm3,Z=2,Dc=1.805mg/m3,μ=2.153mm-1,F(000)=408,R=00553,Rw=0.1732;该化合物是分立结构,是由MoO4四面体簇和Ni(en)3八面体簇形成,其中MoO4四面体簇和Ni(en)3八面体簇交替排列,存在较强的氢键作用,结构中分立的手性配合物Ni(en)3的两种对映体构象以MoO4簇为中心对称排布.
简介:多代替的dihydrofurans是为自然产品和药品的合成的珍贵中介。可观的注意集中于发展有效并且为他们的准备的regioselective方法。把K2CO3用作一个底,与fur-2-oylmethyltriphenylarsonium溴化物1的反应和乙醇2-acetyl-3-arylacrylate2在在房间温度的tetrahydrofuran,我们发现一个有效协议被完成综合trans-3-aryl-4-carbethoxy-2,3-dihydro-2-fur-2-oyl-5-methylfurans3在有高stereoselectivity的好产量。化合物3的结构被红外,1HNMR,MS和HRMS证实。为3的形成的机制被建议。
简介:Onenovelorganic-inorganichybridsupramolecularassemblies|(NDPA)(18-crown-6)]2+(DMA)+·3ClO4-(1),hasbeensuccessfullyconstructedthroughtheprominentstrategiesofcrystalengineering(NDPA=N,N-dimethyI-1,4-phenylenediamine,DMA=dimethylamine),andcharacterizedbyIR,powderXRDandsinglecrystalX-raydiffraction.Inthestructure,thesupramolecularorganiccationsandinorganicClO4-anionsarearrangedalternatelyandlinkedbyN-O…Hhydrogenbonds.ItisworthytonotethattheClO4-arelinkedtoformone-dimensionalinorganicchainthroughstrongNH…Ohydrogenbondsalongb-axis.Thereisnodistinctdielectricanomalyinthetemperaturedependentandfrequency-dependentdielectricconstantcurves,suggestingthatnophasetransitionexistswithinthemeasuredtemperaturerange(120-420K).Therelativedisplacementofcationsandanions,theturnedpolarizationofmolecularelectricmomentandmacrocyclicmoleculerotatorarethemainfactorstodeterminethetrendofdielectricconstant.
简介:归纳了从钛铁矿中分离铁和二氧化钛的方法,包括亚熔盐法、预氧化法、还原锈蚀法;其次,初步总结了目前国内外制备Fe3O4磁性纳米颗粒和TiO2纳米粒子的方法。最后,对Fe3O4/TiO2复合材料的制备方法包括溶胶-凝胶法、微乳液法、均匀沉淀法作了梳理。Fe3O4/TiO2复合纳米材料很好地解决了单独使用TiO2作为废水处理催化剂,在实际应用过程中易随水流失,难以回收利用的问题,具有一定的实用性。
简介:N酰--hydroxy-4-phenyl-oxazolidinethiones能被处理很快在高收益变换成他们的乙醇thiol酉旨与在0è的EtSH
简介:Theoptimalconditionsforthecomplexationreactionofmeso-tetra(3-methoxy-4-hy-droxyphenyl)porphineT(3-M-4HP)Pwithplatinumandrhodiumarepresented.Beer’sLawisobeyedwhentheconcentrationofrhodiumisintherangeof0.45-1.15μg/25mL.Themolarabsorptivityofrhodiumwasfoundtobe1.99×106L·mol-1·cm-1at460nm.ThevalueofεPtwasfoundtobe6.28×105L·mol-1·cm-1bylinearregressionmethod.TheKcoefficientmethodandcompensatingcoefficientwereusedtodetermineplatinumandrhodiumsimultaneoulywithoutremovalormaskingoftheinterferentsinthesample.Theresultsforthedeterminationofplatinumandrhodiuminthemixedsolutionofplatinumandrhodiumaresatisfactory.
简介:采用一步法合成了氨基化四氧化三铁(NH2-Fe3O4)磁性纳米材料,并以XRD,IR等手段对其进行了表征.将NH2-Fe3O4组装到磁性玻碳电极表面,得了NH2-Fe3O4修饰的磁玻碳电极,并以该修饰电极为工作电极,研究了其电化学性能.利用差分脉冲溶出伏安法研究了铅(Ⅱ)离子和铜(Ⅱ)离子在该修饰电极上的电化学行为.结果表明:NH2-Fe3O4纳米粒子可显著提高Pb2+和Cu2+在电极表面的富集量,提高溶出峰电流.由于差分脉冲溶出伏安曲线中Pb2+和Cu2+的溶出峰电位差较大,且没有相互干扰,所以该电极可用于Pb2+和Cu2+的同时测定.