22二甲基联苯44二甲酰氯的合成

2,22224,421,2(1.,300220;2.,300402):2,2224,42,,4,2,22224,4274%,86%:2,22224,42;;:TQ242:A:1003-5214(1999)05-0021-032,22224,42[1,2],2,22224,42,,,,[3]2,22224,42,,,,4:H2NCH3NH22HClH3CNaNO2PH+I2-NaIPCH2Cl2ICH3IH3CKCNPDMFPd(OAc)2(1)NCCH3CNH3CKOHPO(CH2CH2OH)2H+PH2OHOCOCH3COOHH3CSOCl2ClCOCH3COClH3C(2)(3)(4)11.1IR-400,DMX-300,11062,22224,421.22,2224,42(1)28.5g(0.1mol)2,22224,42250ml30ml,14.3g(0.207mol)40ml,5,:60g(0.24mol),60g(014mol),100ml200ml,,,5,3h48h800ml,,,145146P617Pa3211g,74%,98IR(cm-1):125,:2,22224,42:1998-12-27©1994-2008ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(CDCl3),:211(s,6H),619712(d,2H),7.8(d,4H)1.32,2224,42(2)2117g(0.05mol)1,13g(012mol)KCN,015gKOH100mlDMF200ml,Pd(OAc)2400mg145,,5h500mlw(NaOH)=10%,,10g,86%,113IR(cm-1):2225,1602,1479,10061H2NMR(CDCl3),:2.1(s,6H),7.27.4(d,2H),7.67.8(d,4H)1.42,22224,42(3)9g(0.039mol)2,8.6gKOH75ml,,6h,800ml,,,,10g,98%,328330IR(cm-1):1693,1605,1426,13061H2NMR(DMSO-D6),:2.1(s,6H),7.37.4(d,2H),7.98.1(d,4H)1.52,22224,42(4)15g(0.056mol)390ml(1.24mol),2DMF,,5h,13.8g,80%,9293IR(cm-1):1735,1605(C16H12O2Cl2):(%):C62.56,H3.94;(%):C62.60,H4.0322.1,,,,,,,,,5,,,2.2KCN,,,,,,,,,4,,,:[1]RogersHG.Para2linkedAromaticThermotropicPolyesterswithLowMesophaseTemperature[J].Macromolecules,1987,20:2374.[2]SchmidtHW.InfluenceofLateralSubstituentsonThermalBehaviorandSolubilityofAromaticLC2Polyesters[J].MakromolChem,SympEd,1989,26:47.[3]Christen.GrundlagenderOrganischenChemie[M].Frankrurt:OttoSalleVerlag,1985.726,750.:(1953),,197919861987,,Synthesisof2,22Dimethylbiphenyl24,42dicarbonylDichlorideGUODa2jian1,LIHong2yu2(1.TianjinSyntheticMaterialInstitute,Tianjin300220,China;2.DepartmentofEnvironmentalEngineering,TianjinProfessionalCollege,Tianjin300402,China)22FINECHEMICALS199916©1994-2008ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.