简介:利用水热工艺,选用有机配体3,3’,5,5’-四甲基-4,4’-联邻二氮杂茂(H2X)和CuCl2·2H2O为起始原料,合成了1个新的多酸基杂化化合物[Cu2(H2X)2(Mo6O19)]·2H2O被合成.采用X-射线单晶衍射、红外光谱、元素分析和热重分析等手段对该化合物的结构进行了表征.单晶测试结果表明该化合物为1D链状化合物,属于三斜晶系,P-1空间群,晶胞参数a=0.9469(3)nm,b=0.9544(3)nm,c=2.0599(6)nm,α=90.717(4)°,β=93.518(5)°,γ=102.802(4)°,V=1.8112(9)nm3,Z=4,R1=0.0829,wR2=0.1512.
简介:利用基团拼合原理,将2,2′-联吡啶和硫醚结构引入到1,3,4-噁二唑母体结构中.以1,10-菲罗啉为原料,经过氧化、酯化、肼解以及环合等化学反应,合成了中间体2,2′-联吡啶-3,3′-二甲酰肼、2,2L联吡啶-3,3,-二(5-E1,3,4-噁二唑-2-硫酮])以及4个2,2L联吡啶-3,3′-二(5-E1,3,4-噁二唑-2-硫醚])系列目标化合物,其结构通过1HNMR和单晶X-射线衍射等进行表征.晶体结构分析表明:2,2′-联吡啶的3和3′位上取代基不同,2个吡啶环所在平面的偏转角度不同,1,3,4-噁二唑-2-硫醚结构能使2个吡啶环呈现较大的偏转角度.
简介:Theeffectandmechanismofcarmustine(BCNU)combinedwithall-transretinoicacid(ATRA)ontheapoptosisofhumanglioblastomaU251cellswereinvestigatedbymeansof3-(4,5-dimethylthiazol-2-yl)-2,5-diphe-nyltetrazoliumbromide(MTT)assay,flowcytometry,reversetranscription-polymerasechainreaction(RT-PCR)andWesternblotanalysis.TheresultsshowthatBCNUorATRAshowstime-anddose-dependentinhibitioneffectsonhumanglioblastomaU251cellsandthecombinationofBCNUwithATRAshowsansynergisticinhibitioneffectonhumanglioblastomaU251cells,andthecombinedBCNUandATRAcansignificantlyinhibittheproliferationofhumanglioblastomaU251cells,andinducetheapoptosisofthem,makingthecellsarrestinthestageofG1phase,thestageofSandG2phasesdecline,therateoftheapoptosisofhumanglioblastomaU251cellsincrease,thecorrespondingmRNAexpressionofcyclinEandcyclin-dependentkinase2(CDK2)downregulatedandthecorrespon-dingmRNAexpressionofp27kip1unregulated.Inaddition,thecombinedBCNUandATRAreducedtheproteinexpressionofnuclearfactorkappaB(NF-κB).Takentogether,theseresultssuggestthatthetreatmentofhumanglioblastomaU251cellswithacombinationapplicationofATRAandBCNUcanexertsynergisticeffect,thecourseofthiskindofcombinationchemotherapymaylikelybeassociatedwithmultiplemolecularmechanismsforapoptosis,furthermore,thecyclinEandp27kip1shouldbeconsideredasnoveltargetsforcontrollingthegrowthofglioblastomacells.
简介:Anefficientandenvironmentallyfriendlyprocedurefortheone-potsynthesisoftetrahydropyrimidinonesfromaldehydes,β-diketonesandurea/thioureabyusingmagnesiumbromideasaninexpensiveandeasilyavailablecatalystundersolvent-freeconditionswasdescribed.ComparedwiththeclassicalBiginellireactionconditions,thisnewmethodhastheadvantageofgoodtoexcellentyields(74%-94%)andshortreactiontime(45-90min).ThestructureoftheBiginellireactionproductfromβ-diketone,salicylaldehydeandureahasbeenproposedtopossessanoxygen-bridgebycyclization(intramolecularMichael-addition).
简介:[Co3(1,2-S2C6H4)3(PPh3)3][CoBr3(DMF)].sol(1,sol=CHCl3,O(C2H5)2,H2O)wasobtainedfromthereactionofCoBr(PPh3)3withNa2(S2C6H4)inchloroform.TheCo3coreinthecationof1exhibitsametal-metalbondedisoscelestriangle,inwhichthetwolongerCo-CobondsarebothbridgedbyS2C6H4ligandsontwosidesofthetriangleplanerespectively,whilethebottomshortCo-CobondisbridgedbythethirdbidentateS2C6H4ligand.Aseriesofpolynu-clearcobaltclustercompoundswithphosphine,thiolateand/orsulphurligandswerepreparedbylowoxidationstateCo+withthiolatesinorganicsolvents.Thesetri-,tetra-,hexa-,heptanuclearclustercompounds1-8withvarioustypesofcrystalstructurescanbeviewedasthecondensedpolynuclearcobaltcomplexesthatthecobaltatomframeworkswithsulphurbridgedwerebuiltthroughthesmalltriangularunitsof[Co3S3nL3](n=1,2)withorwithout[CoL](L=PR3,Br,Cl,5-C5H5)fragments.
简介:Poly(4-vinylpyridine)supportednanoparticleofcopper(Ⅰ)iodideisreportedasagreenandrecyclablecatalystfortheregioselectivesynthesisof1,4-disubstituted-1H-1,2,3-triazolesfrombenzylhalides,sodiumazideandterminalalkynesinwater.Thiscatalystcanberecoveredbysimplefiltrationandrecycledupto8consecutiverunswithoutanylossofitsefficiency.
简介:6/3-(4-Chlorophenyl)-s-triazolo[3,4-b][1,3,4]thiadiazoles(2a-e)and(5a-e)weresynthesizedrespectivelybyintermolecularcyclizationof5-aryl/4-chlorophenyl-4-amino-3-mercapto-1,2,4-triazoles(1a-e)and(4)with4-chlorobenzoicacid/arylacids,whichwerecondensedwithpiperazineunderphasetransfercatalystTBABtoyieldthecorrespondingfreebasesofmonopiperazinederivativesandfollowedtoformwater-solublesalts(3a-e)and(6a-e)withhydrochloricacidingoodyields.Theinvitrobiologicalresultsshowedthatpiperazinegroupconjugatedwiththeabovefusedheterocyclesplayedanimportantroleinantibacterialactivity.ThestructuresofnovelcompoundswereconfirmedbyIR,1HNMR,MSandelementalanalysis.
简介:4-(Succinimido)-1-butanesulfonicacidasanefficientandreusableBronstedacidcatalyzedthesynthesisofpyrano[4,3-b]pyranderivativesundersolvent-freeconditions.Thecatalystcanbepreparedbymixingsuccinimideand1,4-butanesultonethatismoresimpleandsaferthanthepreparationofsuccinimidesulfonicacid.Thismethodhastheadvantagesofhighyield,cleanreaction,simplemethodologyandshortreactiontime.Thecatalystcouldberecycledwithoutsignificantlossofactivity.
简介:Achiralrutheniumcomplex[(1S,2S)-DPEN]-RuCl_2(PPh_3)_2(DPEN=1,2-diphenylethylenediamine,PPh_3=triphenylphosphine)wasencapsulatedinthechannelofAl-MCM-41byelectrostaticadsorptionand1,1-dichlorosilacyclobutanemodification.Thepreparedheterogeneouscatalystshowedthesamecatalyticactivityandenantioselectivityasthecorrespondinghomogeneouscatalystintheasymmetrichydrogenationofacetophenone,andcouldbereusedatleastseventimeswithoutsignificantlossofcatalyticactivityandenantioselectivity.
简介:Asurface-renewabletris(1,10-phenanthroline-5,6-dione)iron(Ⅱ)hexafluorophosphate(FePD)modifiedcarbonceramicelectrodewasconstructedbydispersingFePDandgraphitepowderinmethyltrimethoxysilane(MTMOS)basedgels.TheFePD-modifiedelectrodepresentedpH-dependentvoltannetricbehavior,anditspeakcurrentswerediffusion-controlledin0.1mol/LNa2SO4+H2SO4solution(pH=0.4).Inthepresenceofiodate,clearelectrocatalyticreductionwaveswereobservedandthusthechemicallymodiffiedelectrodewasusedasanamperometricsensorforiodatencommonsalt.Thelinearrange,sensitivity,detectionlimitandresponsetimeoftheiodatesensorwere5×10^-6-1×10^-2mol/L,7.448μA·L/mmol,1.2×10^-6mol/Land5s,respectively.Adistinctadvantageofthissensorisitsgoodreproducibilityofsurface-renewalbysimplemechanicalpolishing.
简介:The2-C,methylenegroupof1-aroyl-1,2-dihydro-3H-naphtho[2,1-b]pyran-3-ones(2)havebeenshowedtopossessasuperiorreactivitytowardsmanyoforganicreagents.Thena-phthopyrones(2)condensedwitharomaticaldehydestogivethe2-arylidinederivatives(3).Bromin-ationof2gave1,2-dibromo(4)or5-bromo(5)derivativesdependingonthereactionconditions.Thebasecatalyzedadditionorcycloadditionofnaphthopyrones(2)to4-methoxybenzalacetophenonegavetheexpectedMichaeladduct(6)orthecyclicadducts(7-9)dependingonthetypeofcatalyticbaseandreactionconditions.Structuresoftheproductshavebeenestablishedbyelementalanalyses,IRand~1HNMRspectroscopicmethods.
简介:Anovelaciddyeacidwassynthesizedbythecondensationreactionbetweenbromamineacidand2-amino-6-nitrobenzothiazoleanditsanti-UVprotectionpropertieswereevaluated.Theresultsshowedthatsilkdyedwiththisdyehadverygoodultravioletradiationprotectioncapabilityandexcellentdyeingperformance.TheUV-absorptionmechanismofthisdyewasalsodiscussed.
简介:Alariatcrownetherligand7,16-bis(2-hydroxy-5-methylbenzyl)-1,4,10,13-tetraoxa-7,16-diazacyclooctadeeane(L1)hasbeenpreparedviaone-potMannichreaction.Itscopper(Ⅱ)complexCu-L1wassynthesizedandcharacterizedbyelementalanalysis,IRandUV-visiblespectroscopy.ThecrystalstructureofthecomplexhasbeendeterminedbyX-raydiffractionanalysis.Theresultshowsthatthecopper(Ⅱ)ionissix-coordinatedbytwonitrogenandfouroxygenatoms,twofromthecrownetherandtheothertwofromthedeprotonatedphenolateanions,forminganelongatedoctahedralcomplex.ElectrochemicalstudyindicatesthatthecomplexundergoesreversiblereductioninDMFsolution.
简介:以1,3-丁二醇、柠檬酸为原料,设计、合成了以1,3-丁二醇为核心的柠檬酸-1,3.丁二醇-柠檬酸(cBc)爪状物小分子;再用酯化反应依次与带有功能化集团的硬酯酸、十六醇接枝合成了多元酯类爪形大分子柠檬酸-1,3-丁二醇-柠檬酸-硬酯酸-十六醇(CBC-SH).采用核磁共振、红外光谱对合成的两种化合物进行了结构表征,表明合成的CBC和CBC-SH与所设计的分子结构相吻合.元素分析确定了CBC和CBC-SH的化学组成依次为C16H22O14和C98H184O15.合成的CBC-SH溶于非极性的有机溶剂,不溶于水.将CBC-SH按600μg/g的加剂量添加到不同的轻柴油中,柴油的冷滤点可降低6℃.