合成头孢泊肟酯中间体的气相色谱跟踪分析

:100128689(2003)0620344203(,321004):1212,12,GC2MSSE254(30m0153mm0125Lm)126113%,129514%,128715%,,:;;12;12;12;:R917:A:2003201213:2003202222:,,1944,1[1](cefpodoximeproxetil,cs807),(cefpodoxime,CPDX),,,,,121212,::12::1212::1212[2]:PTC:12[2],,(1)(3)SE254FID,(4)(HPLC)[3],1244320036286©1995-2004TsinghuaTongfangOpticalDiscCo.,Ltd.Allrightsreserved.,,22,,12,,(Bu4NBr),(C15H17N5O6S2)()6910%22.18810,C2R3A,FTDBRUKERAvance400(TMS,CDCl3)QP1000AGCöMS2.2SE254(30m0153mm0125Lm),:0102Mpa;:01025Mpa;:0103Mpa012Ll::30(5min)(15ömin)200(5min),:200:80,:1502.3(GC2MS),,GC2MSGC1GC2MS,(),1212,4122,1()12122212,142412,31()GC2MS,121:();2:12;3:;4:121GC2MS1:();2:12;3:;4:122GC1H2NMR(D6172D4191D2119D1130),D6172(,1);D4191(,1);D2119(,3);D1130(,6)GC2MS1212GC2MS()33.11212(,118119),22(,155156)(,9395)543©1995-2004TsinghuaTongfangOpticalDiscCo.,Ltd.Allrightsreserved.,,,,123112%6113%,6113%3.212124613%7510%8611%9018%9514%,3.312(),12(),12(),112,,4(1)126113%,SE25412,,,,,1(n=2,%)1231194441.021.233.7194638.921.335.62201818.01.6764.5201919.71.4264.4322951.313.9785.722961.324.1086.0322970.633.5087.5322980.633.4887.631:;2:12;3:12,SE254,,,240,1Ll(2)12,80,,9514%128716%(3)12,,,8716%,,(4)121222122212,12,,,,80(5)SE254,,122,,,,,,[1]GongP,WangC,LiW.SynthesisofthesidechainofcefpodoximeproxetilTheprepartionof12chloroethyllsopropylcarbonate[J].ShenyangPharmaSciUniv,1998,15(2):206[2]GenBen2maoren,ShanZhong2jizi,XiaoSong2xiongyi.12Ȇ‚ˍˈ™¦Ë,TeKai2ping6272965,PingCheng6(1994)315[3]LinL,GuanQM.QuantitativeanalgsisofcefpodoximeproxetilbyHPLC[J].GuangdongPharmaSciUniv,2000,16(3):189(382)64320036286©1995-2004TsinghuaTongfangOpticalDiscCo.,Ltd.Allrightsreserved.[29]DoumithM,LegrandR,LangC,etal.InterspeciescomplementationinSaccharopolysporaerythraea:eluci2dationofthefunctionofoleP1,oleG1andoleG2fromtheoleandomycinbiosyntheticgeneclusterofStreptomycesantibioticusandgenerationofnewerythromycinderiva2tives[J].MolMicrobiol,1999,34(5):1039[30]KealeyJT,LiuL,SantiDV,etal.Productionofapolyketidenaturalproductinnonpolyketide2producingprokaryoticandeukaryotichosts[J].ProcNatlAcadSciUSA,1998,95(2):505(346)GCtrackinganalysisofsynthesisoftheintermediateofthecefpodoximeproxetilLiSi2jiao(AcademyofLifeandEnvironmentalSciences,ZhejiangNormalUniversity,ZhejiangJinhua321004)ABSTRACTInthispaperthequantitativeandqualititativeanalysesfortrackingofsynthesisof12chloroethylchloroformate,12chloroethylisopropylcarbonateand12iodoethylisopropylcarbonate,theinterme2diatesofthecefpodoximeproxetil,weredescribedusingGC2MS,1H2NMRandcapillarycolumnGC.Experi2mentsshowedthatthemethodhadgoodresolutionandhighreproducibility.KEYWORDSGaschromatography;Capillarycolumn;12chloroethylchloformate;12iodoethyliso2propylcarbonateester;12iodoethylisopropylcarbonateester;Intermediatesofcefpodoximeproxetil(366)81154%,80100%and72137%,Whiletheadversedrugreactionrateswere6115%,10177%,16192%,7169%,13185%respectively.ConclusionItwasconcludedthatlevofloxcinwasthemosteffectiveandtheleastadversedrugreactionquinoloneandsuggestedasthedrugofchoiceinthetreatmentofsenilepul2monaryinfection.KEYWORDSBacterialpulmonitis;Quinolone;Clinicalefficacy(gatifloxacin),2001,20031,:,:(1),;(2)(20031,E2mail);(3):20031231:()18,,:610051:(1);(2);(3),:1(2000),3(1000),10(500)28320036286©1995-2004TsinghuaTongfangOpticalDiscCo.,Ltd.Allrightsreserved.