
heappearanceofthe1HNMRsignalsofproticsamplesinaproticsolventsdependscriticallyontheconcentrationofthesample.The-OH,-NH2or-COOHsignalscanhavechemicalshiftvaluesandlinewidthsoverawiderangeduetovaryingextentsofhydrogenbondingandchemicalexchange.TheconcentrationcanalsodeterminewhetherornotoneisabletoobserveJcouplingbetweenand-OHprotonandotherprotonsinthesample.Anexampleofthisisillustratedbelow.Thefigu...[
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NMRusersareveryfamiliarwiththeadvantagesofprotondecouplingwhenobserving13C.The13CNMRspectraofphosphoruscontainingcompoundscanbemadesimplerbyapplying31Pdecouplingeitheronitsownorinadditiontoprotondecoupling.Thefigurebelowshowsthe13CNMRspectrumofdimethylmethylphosphonatewithallpossiblecombinationsofprotonand31Pdecoupling.Thedatacollectionrequiredatripleresonanceprobewiththeappropriatebandpassfilters...[
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【英文名称】DibutyltinOxide【分子式】C8H18OSn【分子量】248.92【CA登录号】[818-08-6]【缩写和别名】DBTO【结构式】(CH3CH2CH2CH2)2SnO【物理性质】mp>300oC,溶于大多数有机溶剂,常常在苯、甲苯或者CH3OH溶液中使用。【制备和商品】该试剂在国外大型化学试剂公司有销售。由于具有较高的毒性,建议不要在实验室制备。【注意事项】该试剂由于具有C-Sn键而具有较高的毒性,建议在通风[
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本维莫德是一种小分子芪类化合物,最初是由一种土壤线虫共生菌的代谢产物中分离得到,属于天然产物的范畴,目前完全可以通过人工合成获得;同时也是全球首个芳香烃受体激动剂。2019年5月在我国获批上市;2022年5月在美国获批上市。本维莫德是我国近十年(2012年到2022年)批准上市的三款firstinclass创新药之一,也是目前为止首款先在我国批准上市,然后才被美国FDA批准上市[
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常用的酚羟基保护基有:(1)烷基保护基,比如甲基,叔丁基或三苯基甲基;(2)苄基类保护基,比如Bn或者PMB;(3)烯丙基;(4)硅类保护基,比如TBS;(5)酰基保护基,比如乙酰基或苯甲酰基;(6)MOM保护基;(7)THP保护基;(8)SEM保护基;(9)二甲胺磺酰基;(10)烷氧羰基等等。酚羟基各类保护基如何脱保护。总体来说可以分为如下:(1)酸脱保护,上图中的例[
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Whenmanychemistsareaskedwhatisthe2JH-Hcouplingforcompoundslikemethane,acetone,methylenechloride,dimethyletherorDMSO,theywilloftenreturnalookofconfusion."Thereisnocoupling,"theywillsay,"theprotonspectrumisasinglet".Indeedtheprotonspectrumisasingletforthesecompoundsbut2JH-Hisnotequaltozero.Theonlyreasonthatthecouplingisnotobservedinthespectrumisbecausethechemicalshiftsofeachproto...[
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Manypeopleusestatementslike,"ItisfastontheNMRtimescale"withoutreallyhavinganunderstandingofwhatthe"NMRtimescale"means.Assumewehaveacompoundwithtwointer-convertibleconformations,AandB,eachofwhichgivesadifferentNMRspectrum.IftheinterconversionbetweenAandBisveryslowthenweexpecttogetaspectrumwithbothconformationsAandBresolved.Iftheinterconversionisveryfastthenwewouldgetanunresolved...[
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ItisveryimportantthatyourNMRsamplesaremixedwellbeforeNMRdataareacquired.Ifthesamplehasaconcentrationgradient(i.e.moreconcentratedatoneendofthesamplecolumncomparedtotheother)itwillbeverydifficulttoshimthemagnetovertheentirevolumeofthesampleasthemagneticsusceptibilityisnotconstantoverthesamplevolume.AsaresulttheNMRlinesmaybeskewedandwillbemuchbroaderthannecessary.Thiswillleadtoamuchlowersignal-to-no...[
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二乙氨基三氟化硫(DAST)是有机合成中被广泛应用的氟化试剂,它是(二烃基氨基)三氟化硫家族中的一个成员。DAST属于亲核型氟化试剂,它能够将醇羟基转化成为相应的氟,将醛酮转化成为偕二氟化物[1]。DAST将伯醇转化成为相应氟化物的反应可以在非常温和的条件下进行。通常在–78oC下加料来抑制最初的放热过程,然后让反应自动升至室温片刻即可(式1)[2,3]。仲醇的反应虽然[
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