简介:Benzodiazepineandbenzothiazepinederivativeshavebeenwellknownastherapeuticallyimportantcompounds.Fournewtricyclicheterocycliccompounds,3a,4,5,11-tetrahydro-3H-1,2,4-triazolo[4,3-d][1,5]benzothiazepines(3),3a,4,5,11-tetrahydro-3H,6H-1,2,4-triazolo[4,3-d][1,5]benzodiazepine(4),3a,4,5,11-tetrahydro-1,2,4-oxadiazolo[4,5-d][1,5]benzothiazepines(5,6)and3a,4,5,11-tetrahydro-6H-1,2,4-oxadiazolo[4,5-d][1,5]benzodiazepines(7,8),havebeensynthesizedby1,3-dipolarcycloadditionreactionsof2,3-dihydro-1,5-benzothiazepinesand2,3-dihydro-1H-1,5-benzodiazepinewithbenzonitrileN-phenylimineandbenzonitrileoxides,respectively.Theconformationsofsomecycloadductsandcycloadditionmechanismaredescribed.
简介:Anovelseriesofpyrido[1,2-e]purin-4(3H)-onederivativescontainingpolarsubstituentson5'-positionweredesignedandpreparedaspotentialPDE5inhibitors.Thispaperreportsthesyntheticroutes,1H-NMRdata,andthePDE5inhibitoryactivitiesofthetargetcompounds.Thepolarpiperazinylgroupcontained(on5'-position)compound,3B2,showedthehighestactivityamongthetestedderivativesbutlesspotencythansildenafil1.
简介:利用PCR以实验室构建的原核重组表达质粒pProEX-OCIF为模板扩增得到N末端融合有6×His标签和rTEV蛋白酶识别序列的人破骨细胞形成抑制因子(OsteoclastogenesisInhibitoryFactor,简称OCIF)结构域D1~D6(简称OCIFm)编码基因片段;将其与pMD18-T连接,转化大肠杆菌TOP10,筛选得到阳性重组质粒pMD18-OCIFm,双酶切重组克隆质粒pMD18-OCIFm得到OCIFm基因片段;将其定向插入甲醇营养型酵母分泌表达载体pPIC9中,构建获得重组表达质粒pPIC9-OCIFm.测序验证后,以限制性内切酶SalⅠ线化,电穿孔转化酵母宿主菌GS115.筛选得到阳性表达菌株后,甲醇诱导表达4d,SDS-PAGE和Westernblot对表达情况进行分析和确认.所获得的OCIFm基因片段在甲醇营养型酵母中表达量占菌体总蛋白的30%以上.利用Ni-NTA树脂对表达产物进行一步亲和层析纯化.活性测定表明纯化的表达产物可诱导体外培养的成熟破骨细胞样细胞的凋亡.表达产物的生物学活性较利用原核表达系统明显提高.
简介:RemanspectroscopyisusedasatooltomonitorthereactionbetweenN,N’-di(pmethyl)monothioxamidesand1,3-diaminetrimethyleneandtodetectthereactionintermediate.Byobservingchangesof1024cm-1C=Sbandandappearanceofanewbendataround1720cm-1,thereactionmechanismisdiscussed.
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简介:TwonewintercalationcompoundsFe0.90PS3(phen)0.41(1)(phenstandsfor1,10-phenanthrolineincludingapartof1,10-phenanthrolineH+)andFe0.83PS3(bipy)0.34(2)(bipystandsfor2,2’-bipyridineH+)weresynthesizedbythereactionofthelayeredFePS,with1,10-phenanthrolineor2,2’-bipyridineinthepresenceofaniliniumchloride.Theywerecharacterizedbyelementalanalyses,powderX-raydiffraction(XRD),infraredspectroscopy.Thelatticespacingoftheintercalatewasexpandedby0.90nmforFe0.90PS3(phen)0.41and0.57nmforFe0.83PS3(bipy)0.34withrespecttothepristineFePS3,indicatingthattheringplaneoftheguestsisperpendiculartothelayerofthehost.TheUV-visabsorptionspectraofthefiltrateinpreparationoftheintercalatesindicatethat1,10-phenanthrolineor2,2’-bipyridinealsoactsasacomplexingagenttoremoveintralamellarFe2+ionsintothesolutionduringintercalation.Themagneticpropertiesof1and2werestudied.
简介:Twocystine-bearing1,3-bridgedcalix[4]areneswereusedasthecoatingsofthequartzcrystalmicrobalance(QCM)withgoldelectrodes.Thetwocalix[4]arenederivativeswereself-assembledontothegoldelectrodesurfacebythecovalentattachmentbetweenthedi-sulfurandgold.Thecompoundofcystine-bearingbi-phenylalanine1,3-bridgedcalix[4]arene(CPC)withlongeralkylchainhadbetterself-assembledcapacityontothefreshsurfacesofgoldelectrodethanthatofcystine-bearing1,3-bridgedcalix[4]arene(CC)withcomparablyshorteralkylchain.ThemodifiedQCMsensorswereusedtorecognizethebutylamineisomersingas.TheresultsshowedthattheQCMcoatedwithbothcompoundshadpreferentialaffinityton-butylamine,theni-butylamine,t-butylamineintherangeoflowconcentrations,indicatingthatintherecognitionprocess,thesterichindranceeffectplayedanimportantrolewhenformingcomplexwithguestmolecules.Whentheconcentrationsoftheanalyteswereincreased,thepolarityandthemagnetismofthebutylaminebecamedeterminativefactors.Thereversibilitywasimprovedgreatlyandtheequilibriumtimewasmuchshorterontheself-assembledfilmthanonthefilmobtainedbydroppingcoating.
简介:Afacilesolidphasesynthesisof2-substituted1,3-oxazin-6-onesusingpolymer-supportedMeldrum'sacidhasbeenreported.Reactionoftheresin-boundcyclicmalonicacidesterwithtriethylorthoformateandsubsequentdoublesubstitutionwithamide,affordedthecorrespondingpolymer-supportedacylaminomethylenecyclicmalonicacidester,whichuponthermaltreatmentledto1,3-oxazin-6-onesingoodyieldsandwithhighpurity.
简介:Anewsyntheticapproachto1,4,6-tri-O-benzylmyo-inositolwasdescribedonthebasisoftheregioselectivebenzylationof1,2-O-isopropylidene-4,6-di-O-benzylmyo-inositol,subsequentacidhydrolysis,phosphorylationwithtetrabenazylpyrophosphateandappropriatedeprotec-tion.
简介:The1.3-dipolarcycloadditionreactionof2-trifluoromethyl-oxazoloneandtheactivatedcarbon-carbonmultiplebondwasstudiedandgaveaconvenientwaytosynthesize2-trifluoromethylpyrrolederivatives.
简介:热行为,机制和在一个规划温度的模式的标题混合物的发热的第一阶段的分解反应的运动参数借助于DSC,TG-DTG和红外被调查了。反应机制被建议。在微分形式,明显的激活精力(Ea)和这反应的pre指数的因素(A)的实验运动模型功能是(1-)?1.119,211.3kj/mol和1020.2s?1分别地。混合物的热爆炸的批评温度是202.2爠慥瑣潩?㈠低??湡敧漠??????????????鈿酌顛鱎?????疞????陴?陴?T
简介:标题化合物C26H26O5以2,3-萘二甲醛和5-甲基-1,3-环己二酮为原料,在醋酸溶剂中,室温下经搅拌多组分一锅法合成得到.其结构通过单晶X-射线衍射法确定,晶体属单斜晶系,空间群P21,相对分子质量Mr=418.47,晶胞参数a=0.99004(8)nm,b=1.09098(9)nm,c=1.04246(11)nm,V=1.08753(17)nm3,Z=2,晶胞密度Dc=1.278g/cm3,吸收系数μ=0.088mm-1,单胞中电子的数目F(000)=444.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R1=0.0533,wR2=0.1293.在晶体结构中新形成的吡喃环为半椅式构象,而茚中五元环则为信封式构象.