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1、Chapter8SpectralAnalysisof2DCorrelationNMRSpectroscopyCommonHomonuclear2D2Dchemicalshiftcorrelationspectroscopy:1.2D1H-1HCOSY(COrrelationSpectroscopY)2.13C-13C2DCorrelations:2D-INADEQUATE(IncredibleNaturalAbundanceDoublEQUantumTransferExperiment)2D1H-1HCOSY(CO
2、rrelationSpectroscopY)2Dchemicalcorrelationspectroscopy)δδXA1ΗδppmAXspinsystem:δAX,AδAX1A2A1X21ΗδppmδXA,XδX2D1H-1HCOSYexperimentstrongFnoiseofCH13symmetrizationofcosydataHorizontalF=0axialpeaks12D1H-1HCOSY90ospectrumofN-methyl-benzosicarbostyril11,514678131213
3、,1211,1213,147,6δΗ6,586,87,8δΗ2D1H-1HCOSY90oexperiment4,625δ1ΗF11δδΗΗ5,45,64,25,2FδΗ26,2symmetrizationt-noise12D1H-1HCOSY90ospectrum413523,445,43,221,23Cδ1Η51δ1Η2D1H-1HCOSY90ospectrumB2aδ1Η2a,e2e2a,1a1a2e,1a52e,1e2a,1e1e1a,e3,45,642a,32e,336a5,6a6e5,6e6a,eδ1Η2
4、D1H-1HCOSY90ospectrum2’4’3’2’,3’5’4’,3’4’,5’6a’5’,6a’δ1Η6e’6a’,e’5’,6e’1’2’,1’Dδ1Η2D1H-1HCOSY90ospectrum910,9110,9‘9‘δ1Η89‘,89,878,71,71079‘918δ1Η2D1H-1HCOSY90ospectrum10δ1Η634‘56,5910,913,46,14,4‘49‘4,510,9‘2‘21,23,22,2‘89‘,89,81044‘9‘951682‘32δ1Η2D1H-1HCOSY4
5、5ospectrumXMAofDibromo-PropionicAcidCOSY90oδ1Ηδ1ΗCOSY45o2JAM3J3MXJAX2D1H-1HCOSY45oexperiment2a2e2J2a,e1aδ1Η1e2J1a,eδ1Ηppm2D1H-1HLong-RangeCOSYoftricyclodecaneδ1Ηo-COSYδ1Η90LR-COSY2J4JABAC3JAI54JJAJ3JBJHJ3JAK4J4J4JJKIKFK2D1H-1HHD-(HomonuclearDecoupling)COSYoftr
6、icyclodecane1ΗδppmJ,JJ,IJ,HJ,JJ,C90oJ,DJ,DJ,CJ,HJ,AJ,IJ,K1ΗδppmJ,BJ,AKJIHDCBAprojectionofF1axis2D1H-1HSE(SpinEcho)-COSYspectrumofDibromo-PropionicAcidMAX1ΗδppmrX,AX,MM,ArδXδMδAA,MM,XA,X2DSECSYspectrumF2(δ)HΔδ/2F1=02D1H-1HDQF-COSY(DoubleQuantumFilteredCorrelati
7、onSpectroscopy)+180oextensionplotAMXpositive&negativecontours-2J1ΗδppmAMF13JMXM,X3J3JAXMXF21Ηδppm2D1H-1HDQF-COSYspectrumδΗ1Ηδppm2D1H-1HDQF-COSYspectraDQF-COSYprojectionF1Ηδppm2COSY90oprojectionF1Ηδppm21HNMRComparisionofDQF-COSYandTQF-COSYspectraDQF-COSYAXTQF-C
8、OSYAX2D1H-1HPH-COSY(Phasesensitivecosy)experimentAββJ+AXX1180oA2αβcrosspeakofF-1βαpureabsorptionphase1AΗδppm1X2ααXdispersivediagnalpeaksF1Ηδppm22D1H-1HPhasesensitiveCOSYspectrumofD