联苯氯甲基化反应的研究

1310Vol.13,No.102005521FineandSpecialtyChemicals121221(1.,200237;2.,201900):,/H2O,,4,422:;;4,42;StudyonChloromethylationofBiphenylFANGQi1,ZHUChun2yan2,RENXiao2li1,XUEZhang2,XIAJian2zhong2,SHENYong2jia1(1.InstituteofFineChemicals,EastChinaUniversityofScienceandTechnology,Shanghai200237,China;2.ShanghaiBaosteelChemicalCo.,Ltd.,Shanghai201900,China)Abstract:4,42Dichloromethylbiphenylwassynthesizedthroughchloromethylationofbiphenyl,startingwithbiphen2ylandparaformaldehydeasrawmaterials,zincchloride/H2Oascatalystinthepresenceofhydrogenchloride.Thefactorssuchasreactiontemperatureandreactiontimeinfluencingonreactionyieldandpuritywerediscussed.AndtheimpuritiesinproductwereanalyzedbyGC2Mass.Keywords:biphenyl;chloromethylation;4,42dichloromethylbiphenyl;paraformaldehyde4,42(4,42bis(chloromethyl)biphenyl,BCMBP),FPCBS2X,,1;2,32060,CIBA4BC2MBP,:,4,42208090,BCMBP5,20,BCMBP6,,,BCMBP,2090BCMBP19977(),8,4,42,52:2005202225:(19802),,,©1994-2008ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(50%);,4,4294%97%,,,/H2O,BCMBP,,,55%,BCMBP1:(HP21101);(BrukerAVANCE500);2(GC8000TOP,FINNIGANVOYAJER):,96%,;2500mL3018g(012mol),(5%)1319g(0144mol),(5%)4812g(01336mol),(99%)4616mL(018mol),16mL,200mL,,(250mL)(500mL),2L,,,,BC2MBP,85%(HPLC)1/5,,HPLC70%BCMBP,2()95%BCMBP,mp136138,50%60%3311,,4011/h/%/h/%14341052110531172640157221054197384516823125814048471212412561205846157252056198610511602620581277105411827255712881054118282557132912531822916121551012541383016141351112551623124231551220561483224261431320541233365541201420561383467531401541919035725816416632199367258176178391843760361671884119038100481801984319839140581432010541204016057164:1145560,15284550,29362530,374010151,2560,50%60%,,,5560,10h,56148%;4550,12h58140%;2530,65h,72h58176%;1520,140h58143%,,60%3124,42,,:,,,62©1994-2008ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.:2,:,4,4242ADE,,ADE,A;,DE(5560),DE,D21%,E18%(2530),DE7%4%(1015),DE216%116%,,,313,HPLC,,22,,,42h1%;A,23h,(48175%),A,,25%4,422/h/%A/%4,42BCMBP/%D/%E/%09615000020131133512528164317471412312561464817530147214441752915316645134371322159418833214741171411842194510642110033170501533120514947150155261995813331855125550141261925716031245157600132251595911831645172:2530,59%DE,1.M.:,2004.17,1482NipponKayakuKabushikiKaisha.Naphthalenering2containingres2ins,resincompositionsandcuredproductsthereofP.US5780571,19982072143NankaiKagakuKogyoKK.Preparationof4,42bis(hydroxymeth2yl)diphenylfrombis(chloromethyl)diphenylP.JP0920851,19972082124NipponKayakuCo.,Ltd.MethodforproducingbiphenyldicarboxylicacidP.JP2001348357,20012122185AmericanViscoseCorporation.4,42bis2(chloromethyl)2biphenylP.US3007975,19672112076UbeIndustries,Ltd.Preparationof4,42bis(chloromethyl)biphen2ylP.JP10139699,19982052267UbeIndustries,Ltd.Manufacturingof4,42bis(chloromethylbi2phenyl)asintermediateforfluorescentbrightenerandepoxyresinP.JP11080047,19992032238UbeIndustries,Ltd.Preparationof4,42bis(chloromethyl)biphen2ylP.JP11130706,19992052189KoreaResInstChemTech.Processforpreparingof4,42bischloro2methylphenylP.KR127251,199820420110,,,.4,42()J.,1997,34(4):363711,,.4,42()J.,1998,7(3):4648,5112,,,.4,42J.,2001,38(3):414272©1994-2008ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.