NMR常見溶劑峰和水峰(共4頁)

1、精選優(yōu)質(zhì)文檔-傾情為你奉上溶劑 1H化學(xué)位移（精細(xì)多重峰數(shù)） JHD/Hz 13C化學(xué)位移（精細(xì)多重峰數(shù)） JCD/HzNMR溶劑中殘余H2O或HOD的質(zhì)子化學(xué)移相對(duì)密度（20） 熔點(diǎn)/ 沸點(diǎn)/ 丙酮d6 2.05(5) 2.2 206.68(13) 29.92(7) 0.9 19.42.8 0.87 -94 57 氯仿-d 7.27(1) 77.23(3) 32.0 1.5 1.50 -64 62 重水 4.80(DSS)4.81(TSP) 4.8 1.11 3.8 101.4 N，N-二甲基甲酰胺-d78.03(1) 2.92(5) 2.75(5 1.9 1.9 163.15(3) 34.

2、89(7) 29.76(7 29.421.021.13.5 1.04 -61 153 二甲基亞砜-d62.50(5) 1.9 39.51(7) 21.03.3 1.18 18 189 甲醇-d44.87(1) 3.31(5) 1.7 49.15(7) 21.44.9 0.89 -98 65 注：JHD為溶劑本身的其他1H對(duì)與之相對(duì)應(yīng)的1H之間的耦合常數(shù)，JCD為溶劑本身1H對(duì)13C的耦合常數(shù)，H2O和交換了D的HOD上的1H產(chǎn)生的即水峰的化學(xué)位移氯仿：小、中小、中等極性DMSO：芳香系統(tǒng)（日光下自然顯色、紫外熒光）。對(duì)于酚羥基能夠出峰。芳香化合物還是芳香甙，都為首選。吡啶：極性大的，特別是皂甙

3、對(duì)低、中極性的樣品，最常采用氘代氯仿作溶劑，因其價(jià)格遠(yuǎn)低于其它氘代試劑。極性大的化合物可采用氘代丙酮、重水等。 針對(duì)一些特殊的樣品，可采用相應(yīng)的氘代試劑：如氘代苯（用于芳香化合物、芳香高聚物） 、氘代二甲基亞砜（用于某些在一般溶劑中難溶的物質(zhì)） 、氘代吡啶（用于難溶的酸性或芳香化合物）等。丙酮：中等極性甲醇：極性大氯仿甲醇：石：乙 5；1小極性石：丙 2：11：1中等極性氯仿：甲醇6：1極性以上 含有一個(gè)糖 2：1 含有兩個(gè)糖含有糖的三萜皂甙：一般用吡啶常見溶劑的化學(xué)位移常見溶劑的1H在不同氘代溶劑中的化學(xué)位移值 mult.氘 代 溶 劑CDCl3(CD3)2CO(CD3)2SOC6D6CD3

4、CNCD3ODD2OC5D5N殘余溶劑峰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.

5、013.073.282.163.343.34C5H5NCH(2),mCH(3),mCH(4),m 8.627.297.688.587.357.768.587.397.798.536.666.988.577.337.738.537.447.858.527.457.878.727.207.57CH3COOC2H5CH3,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,tCH

6、2,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常見溶劑的化學(xué)位移常見溶劑的13C在不同氘代溶劑中的化學(xué)位移值 氘 代 溶 劑CDCl3(CD3)2CO(CD3)2SOC6D6CD3CNCD3ODD2OC5D5N溶劑峰77.16206.2629.8439.52128.061.32118.2649.00-123.44135.43149.84CHCl377.3679.1979.1677.7979.177

7、9.44(CH3)2CO207.0730.92205.8730.60206.3130.56204.4330.14207.4330.91209.6730.67215.9430.89(CH3)2SO40.7641.2340.4540.0341.3140.4539.39C6H6128.37129.15128.30128.62129.32129.34CH3CN116.431.89117.601.12117.911.03116.020.20118.261.79118.060.85119.681.47CH3OH50.4149.7748.5949.9749.9049.8649.50C5H5N149.9012

8、3.75135.96150.67124.57136.56149.58123.84136.05150.27123.58135.28150.76127.76136.89150.07125.53138.35149.18125.12138.27CH3COOC2H521.04171.3660.4914.1920.83170.9660.5614.5020.68170.3159.7414.4020.56170.4460.2114.1921.16171.6860.9814.5420.88172.8961.5014.4921.15175.2662.3213.92CH2Cl253.5254.9554.8453.4

9、655.3254.78n-hexane14.1422.7031.6414.3423.2832.3013.8822.0530.9514.3223.0431.9614.4323.4032.3614.4523.6832.73核磁知識(shí)(NMR)一：樣品量的選擇氫譜，氟譜，碳譜至少需要5mg. 1H-1H COSY, 1H-1H NOESY, 1H-13C HMBC, 1H-13C HSQC需要10-15mg. 碳譜需要30mg.二：如何選擇氘代溶劑常用氘代溶劑: CDCl3, DMSO, D2O, CD3OD.特殊氘代溶劑: CD3COCD3, C6D6, CD3CN。極性較大的化合物可以選擇用D2O或CD3OD，如果想要觀察活潑氫切記不能選擇D2O和CD3OD。CDCl3為人民幣2-