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时间:2020-04-19
《硝酸铜氧化安息香制备苯偶酰.pdf》由会员上传分享,免费在线阅读,更多相关内容在行业资料-天天文库。
1、!"!!!!!!"!研究快报!PREPARATIONOFBENZILBYOXIDIZING"!!!!!!"!BENZOINWITHCUPRICNITRATEWENRuiming(文瑞明),DINGLiangzhong(丁亮中),LUOXinxiang(罗新湘)andYUShanxin(俞善信)(DepartmentofChemistry,HunanCityUniuersity,Yiyang413049,Hunan,China)CLCnumberO625.42DocumentcodeAArticieID0438-1157(2003)01-0135-02Key
2、wordsbenzii,benzoin,cupriccompound,cupricnitrate,oxidationINTRODUCTION1EXPERIMENTALBenziiisanimportantphotosensitiveinitiatoroforganic1.1Reagentsandinstrumentssynthesisintermediates,medicinaiintermediatesandPhCHOHCOPh,Cu(NO3)2·2H2O,CuSO4·5H2O,Cuuitravioietsoiidifiedresin(UVresin),
3、andisusuaiiy(CH3COO)2·H2O,CuCi2·2H2O,C(uOH)2·CuCO3,preparedbyoxidizingbenzoin.TheoxidizersandmethodsCH3COOHareC.P.reportedaremainiy:(PhCHEtN)+Br-(/PhCO)O/2322XRC-1micromeidometer,PE-2400CHNeiementaiMeCN[1],DMSO/(COCi)/CHCi[2],CrO·CHNH·anaiysisinstrument,510Ptypeinfraredspectro-com
4、parator,222332HCi/AiO[3],themetaiiorganiccompound[4],microwaveOP-1000Amassspectrometerandroutineorganicsynthesis23[5]instruments.radiation,etc.Thereactionconditionsofsomemethods1.2Synthesisofbenziiareharsh,thetoxicityisheavy,thereactionreagentisPut2.1g(0.01moi)benzoin,0.033moidiff
5、erentexpensive,thepreparationisdifficuit,theaftertreatmentcoppersaits(theamountofcupricsubcarbonateisreducedistediousortheconversionratioofmateriaisisiow.byhaif),10miaceticacidand5miwaterintoa100miCupriccompoundisakindofweakoxidizer.Uptiiinowthree-neckbottie,instaiiarefiuxcondensi
6、ngtube,heatthereisoniythereportofoxidizingbenzoinwithcupric[6][7]andrefiuxthemixturefor2h,cooi,addwaterandstir,suifate-pyridinewithcupricacetate-aceticacid.Thisputthemixtureinabeakerandieaveitatapaperstudiestheprobiemofoxidizingbenzoinbyusingstandstiii.Thensuctionfiiterwashwithwat
7、ertoneutraitocupricnitrate,cupricchioride,cupricsuifate,cupricobtaintherawproduct.Andthenuse95%ethyiaicohoi-acetateandcupricsubcarbonateasoxidizers.Thewatertorecrystaiiizeandputtheproductinadesiccator.experimentairesuitsindicatethatthesecupriccompoundsAfterdesiccation,aiightyeiiow
8、productisobtained.canaiioxidizebe
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