核磁共振波谱-13CNMR

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1、核磁共振波谱-13CNMR13C-NMR的特点13C-NMR信号于1957年被发现，1970年才开始应用于结构研究。•13C峰度仅1.11％，比1H信号弱得多，约1/5800•化学位移范围：0～220ppm（比氢谱宽将近20倍）•提供各种类型碳（伯、仲、叔、季碳）的信息。•不能用积分曲线获取碳的数目信息（但定性地来讲，二个碳的信号强度一定大于一个碳）•邻近有吸电子基团，信号移向低场（左移）•碳周围电子密度增加，信号移向高场（右移）•常规13CNMR谱中，所有碳信号均为单峰。16Mar2005AcquisitionTime(se

2、c)1.7892CommentB5-O4-Si3-H2Date19/11/200112:50:34Frequency(MHz)No.Atom67.94Nucleus(ppm)13CNo.OriginalPointsCountAtom32768PointsCount(ppm)32768SweepWidth(Hz)18314.44OHNo.1Atom3(ppm)No.Atom72.96(ppm)92'130.021372.9692'130.022284.18106'130.02HOO2284.18106'130.023895.86

3、115158.554696.90124'163.8453108101.301395.869164.65115158.5563'115.69147167.56OH745'6115.691596.905197.86124'163.8481'128.82OHO510101.30139164.6563'115.69147167.5629.7975'115.69155197.8630.0729.5081'128.82206.0530.3629.21TMS115.69(3',5')130.02(2',6')0.0030.6428.9396

4、.90(6)95.86(8)72.96(3)167.56(7)84.18(2)197.86(5)164.65(9)163.84(4')158.55(5)128.81(1')101.30(10)200150100500206.05115.69(3',5')130.02(2',6')167.56(7)197.86(5)164.65(9)163.84(4')158.55(5)128.81(1')20015013C-NMR的测定技术•无畸变极化转移技术(DEPT)–DistortionlessEnhancementbyPolariza

5、tionTransfer–原理：采用脉冲序列，将高灵敏度的1H信号强度转移到13C核上,并测定其13C-NMR谱，改变照射1H的第三脉冲宽度(θ)，使之作45°，90°，135°的变化y–一种特殊技术，可识别碳的类型（CH3,CH2,CH,andC)•θ45°：CH，CH，CH↑y2390°：CH↑，CH消失或很弱(↑)3135°：CH，CH↑；CH↓32–定量性很强，可确定碳的数目QC8-Dept18Apr2002QC8-DMSO-CAcquisitionTime(sec)0.9667CommentQC8-DMSO-Dept

6、DateTueJan2203:40:382002DateStampTueJan2203:40:382002FileNameD:MyDocumentsChemicalNMR500MHzQC8QC8-DMSO-C.dxFrequency(MHz)125.78Nucleus13COriginalPointsCount32768OwnerGUESTPointsCount32768SolventDMSO-D6SweepWidth(Hz)33897.27OH3'OH2'4'39.50HO8O1'5'7926'610354OCH

7、339.66OHO39.8339.162'-C5-C6'-C-OCH32-C4'-C5'-C7-C1'-C8-C=CO9-C3'-C3-C6-C10-C59.6340.0038.99145.20115.7293.55164.08161.24148.66120.55115.3998.51177.86156.30155.56137.63120.77104.1548.5840.091801701601501401301201101009080706050403020100ppmD:MyDocumentsChemicalNMR

8、500MHzQC8QC8-DMSO-C.dx13Jun2002QC19-DeptB4-O8-H2-Si2AcquisitionTime(sec)1.7892CommentB4-O8-H2-Si2DateSatMay1920:25:232001DateStampSatMay