NMR常见溶剂峰和水峰

溶剂1H化学位移δ（精细多重峰数）JHD/Hz13C化学位移δ（精细多重峰数）JCD/HzNMR溶剂中残余H2O或HOD的质子化学移相对密度（20℃）熔点/℃沸点/℃丙酮—d62.05(5)2.2206.68(13)29.92(7)0.919.42.80.87-9457氯仿-d7.27(1)77.23(3)32.01.51.50-6462重水4.80(DSS)4.81(TSP)4.81.113.8101.4N，N-二甲基甲酰胺-d78.03(1)2.92(5)2.75(51.91.9163.15(3)34.89(7)29.76(729.421.021.13.51.04-61153二甲基亚砜-d62.50(5)1.939.51(7)21.03.31.1818189甲醇-d44.87(1)3.31(5)1.749.15(7)21.44.90.89-9865注：JHD为溶剂本身的其他1H对与之相对应的1H之间的耦合常数，JCD为溶剂本身1H对13C的耦合常数，H2O和交换了D的HOD上的1H产生的即水峰的化学位移氯仿：小、中小、中等极性DMSO：芳香系统（日光下自然显色、紫外荧光）。对于酚羟基能够出峰。芳香化合物还是芳香甙，都为首选。吡啶：极性大的，特别是皂甙对低、中极性的样品，最常采用氘代氯仿作溶剂，因其价格远低于其它氘代试剂。极性大的化合物可采用氘代丙酮、重水等。针对一些特殊的样品，可采用相应的氘代试剂：如氘代苯（用于芳香化合物、芳香高聚物）、氘代二甲基亚砜（用于某些在一般溶剂中难溶的物质）、氘代吡啶（用于难溶的酸性或芳香化合物）等。丙酮：中等极性甲醇：极性大氯仿—甲醇：石：乙5；1小极性石：丙2：1——1：1中等极性氯仿：甲醇6：1极性以上含有一个糖2：1含有两个糖含有糖的三萜皂甙：一般用吡啶常见溶剂的化学位移常见溶剂的1H在不同氘代溶剂中的化学位移值mult.氘代溶剂CDCl3(CD3)2CO(CD3)2SOC6D6CD3CNCD3ODD2OC5D5N残余溶剂峰7.262.052.507.161.943.314.797.207.578.72水峰brs1.562.843.330.402.134.874.794.96CHCl3s7.268.028.326.157.587.90(CH3)2COs2.172.092.091.552.082.152.22(CH3)2SOs2.622.522.541.682.502.652.71C6H6s7.367.367.377.157.377.33CH3CNs2.102.052.071.551.962.032.06CH3OHCH3,sOH,s3.491.093.313.123.164.013.073.282.163.343.34C5H5NCH(2),mCH(3),mCH(4),m8.627.297.688.587.357.768.587.397.798.536.666.988.577.337.738.537.447.858.527.457.878.727.207.57CH3COOC2H5CH3,sCH2,qCH3,t2.054.121.261.974.051.201.994.031.171.653.890.921.974.061.202.014.091.242.074.141.24CH2Cl2s5.305.635.764.275.445.49n-hexaneCH3,tCH2,m0.881.260.881.280.861.250.891.240.891.280.901.29C2H5OHCH3,tCH2,q1.253.721.123.571.063.440.963.341.123.541.193.601.173.65常见溶剂的化学位移常见溶剂的13C在不同氘代溶剂中的化学位移值氘代溶剂CDCl3(CD3)2CO(CD3)2SOC6D6CD3CNCD3ODD2OC5D5N溶剂峰77.16206.2629.8439.52128.061.32118.2649.00-123.44135.43149.84CHCl377.3679.1979.1677.7979.1779.44(CH3)2CO207.0730.92205.8730.60206.3130.56204.4330.14207.4330.91209.6730.67215.9430.89(CH3)2SO40.7641.2340.4540.0341.3140.4539.39C6H6128.37129.15128.30128.62129.32129.34CH3CN116.431.89117.601.12117.911.03116.020.20118.261.79118.060.85119.681.47CH3OH50.4149.7748.5949.9749.9049.8649.50C5H5N149.90123.75135.96150.67124.57136.56149.58123.84136.05150.27123.58135.28150.76127.76136.89150.07125.53138.35149.18125.12138.27CH3COOC2H521.04171.3660.4914.1920.83170.9660.5614.5020.68170.3159.7414.4020.56170.4460.2114.1921.16171.6860.9814.5420.88172.8961.5014.4921.15175.2662.3213.92CH2Cl253.5254.9554.8453.4655.3254.78n-hexane14.1422.7031.6414.3423.2832.3013.8822.0530.9514.3223.0431.9614.4323.4032.3614.4523.6832.73核磁知识(NMR)一：样品量的选择氢谱，氟谱，碳谱至少需要5mg.1H-1HCOSY,1H-1HNOESY,1H-13CHMBC,1H-13CHSQC需要10-15mg.碳谱需要30mg.二：如何选择氘代溶剂常用氘代溶剂:CDCl3,DMSO,D2O,CD3OD.特殊氘代溶剂:CD3COCD3,C6D6,CD3CN。极性较大的化合物可以选择用D2O或CD3OD，如果想要观察活泼氢切记不能选择D2O和CD3OD。CDCl3为人民币2-3元，D2O为人民币6元，DMSO为人民币10元，CD3OD为人民币30元。Solvent化学位移(ppm)水峰位移(ppm)CDCl37.261.56DMSO2.503.33CD3OD3.314.87D2O4.79CD3COCD32.052.84