1HNMR Data
pr ot onmu lt CDCl(CD)CO (CD)SO CDCDCNCDODDO3323266332
solvent residual pea k7.262.052.507.161.943.314.79H Os1.562.843.330.402.134.87aa2acetic acidCH s2.101.961.911.551.961.992.083acetoneCH s2.172.092.091.552.082.152.223acet on itrileCH s2.102.052.071.551.962.032.063benzeneCHs7.367.367.377.157.377.33tert-butyl alcoholCH s1.281.181.111.051.161.401.243cOH s4.191.552.18tert-butyl methyl etherCCH s1.191.131.111.071.141.151.213OCH s3.223.133.083.043.133.203.223bBH TArHs6.986.966.877.056.976.92cOH s5.016.654.795.20Ar CH s2.272.222.182.242.222.213Ar C(CH )s1.431.411.361.381.391.4033chloroformCHs7.268.028.326.157.587.90cyclohexaneCH s1.431.431.401.401.441.4521,2-dichloroethan eCH s3.733.873.902.903.813.782dichloromethaneCH s5.305.635.764.275.445.492diethyletherCH t , 71.211.111.091.111.121.181.173CH q, 73.483.413.383.263.423.493.562diglym eCH m3.653.563.513.463.533.613.672CH m3.573.473.383.343.453.583.612OCH s3.393.283.243.113.293.353.3731,2-dim eth oxyethan eCH s3.403.283.243.123.283.353.373CH s3.553.463.433.333.453.523.602dimethylacetamideCH COs2.091.971.961.601.972.072.083N CH s3.023.002.942.572.963.313.063N CH s2.942.832.782.052.832.922.903dim ethylformamideCHs8.027.967.957.637.927.977.92CH s2.962.942.892.362.892.993.013CH s2.882.782.731.862.772.862.853dim eth yl su lfoxideCH s2.622.522.541.682.502.652.713dioxan eCH s3.713.593.573.353.603.663.752ethan olCH t , 71.251.121.060.961.121.191.173CH q, 73.723.573.443.343.543.603.65d2c,dOHs1.323.394.632.47ethyl acetateCH COs2.051.971.991.651.972.012.073CH CH q, 74.124.054.033.894.064.094.1423CH CH t , 71.261.201.170.921.201.241.2423ethyl m ethyl ketoneCH COs2.142.072.071.582.062.122.193CH CH q, 72.462.452.431.812.432.503.1823CH CH t , 71.060.960.910.850.961.011.2623eeth ylen e glycolCHs3.763.283.343.413.513.593.65“gr ea se” CH m0.860.870.920.860.88f3CH br s1.261.291.361.271.292n -h exan eCH t0.880.880.860.890.890.903CH m1.261.281.251.241.281.292H MP ACH d, 9.52.652.592.532.402.572.642.61g3m ethan olCH s3.493.313.163.073.283.343.34h3c,hOHs1.093.124.012.16nitromethaneCH s4.334.434.422.944.314.344.403n -pentan eCH t , 70.880.880.860.870.890.903CH m1.271.271.271.231.291.2922-propanolCH d, 61.221.101.040.951.091.501.173CHsep, 64.043.903.783.673.873.924.02pyr idineCH (2)m8.628.588.588.538.578.538.52CH (3)m7.297.357.396.667.337.447.45CH (4)m7.687.767.796.987.737.857.87silicone gr easeCH s0.070.130.290.080.103tetrahydrofuranCH m1.851.791.761.401.801.871.882CH Om3.763.633.603.573.643.713.742tolueneCH s2.362.322.302.112.332.323CH (o/ p)m7.177.1-7.27.187.027.1-7.37.16CH (m )m7.257.1-7.27.257.137.1-7.37.16triethylamineCH t ,71.030.960.930.960.961.050.993CH q, 72.532.452.432.402.452.582.572
CNMR Data 13
CDCl(CD)CO(CD)SOCDCDCNCDODDO332326633277.16 ?0.0629.84 ?0.0139.52 ?0.06128.06 ?0.021.32 ?0.0249.00?0.01 0.13118.26? 0.02206.26 ?a cet ic a cidCO175.99172.31171.93175.82173.21175.11177.21CH 20.8120.5120.9520.3720.7320.5621.033a cet on eCO207.07205.87206.31204.43207.43209.67215.9430.9230.6030.5630.1430.9130.6730.89CH 3a cet on itr ileCN116.43117.60117.91116.02118.26118.06119.681.891.121.030.201.790.851.47CH 3ben zen eCH128.37129.15128.30128.62129.32129.34tert-but yl a lcoh olC69.1568.1366.8868.1968.7469.4070.3631.2530.7230.3830.4730.6830.9130.29CH 3OCH tert-but yl m eth yl eth er49.4549.3548.7049.1949.5249.6649.373C72.8772.8172.0472.4073.1774.3275.6226.9927.2426.7927.0927.2827.2226.60CCH 3BH TC(1)151.55152.51151.47152.05152.42152.85C(2)135.87138.19139.12136.08138.13139.09CH (3)125.55129.05127.97128.52129.61129.49C(4)128.27126.03124.85125.83126.38126.1121.2021.3120.9721.4021.2321.38CH Ar3CH C30.3331.6131.2531.3431.5031.153C34.2535.0034.3334.3535.0535.36ch lor oformCH77.3679.1979.1677.7979.1779.44cycloh exan e26.9427.5126.3327.2327.6327.96CH 2CH 1,2-dich lor oethan e43.5045.2545.0243.5945.5445.112CH dich lor om ethan e53.5254.9554.8453.4655.3254.782CH dieth yl eth er15.2015.7815.1215.4615.6315.4614.773CH 65.9166.1262.0565.9466.3266.8866.422CH diglym e59.0158.7757.9858.6658.9059.0658.673CH 70.5171.0369.5470.8770.9971.3370.052CH 71.9072.6371.2572.3572.6372.9271.632CH 1,2-dim eth oxyethan e59.0858.4558.0158.6858.8959.0658.673CH 71.8472.4717.0772.2172.4772.7271.492CH dim eth yla cetam ide21.5321.5121.2921.1621.7621.3221.093CO171.07170.61169.54169.95171.31173.32174.57N CH 35.2834.8937.3834.6735.1735.5035.033N CH 38.1337.9234.4237.0338.2638.4338.763dim eth ylformam ideCH162.62162.79162.29162.13163.31164.73165.53CH 36.5036.1535.7335.2536.5736.8937.543CH 31.4531.0330.7330.7231.3231.6132.033CH dim eth yl su lfoxide40.7641.2340.4540.0341.3140.4539.393CH dioxan e67.1467.6066.3667.1667.7268.1167.192CH ethan ol18.4118.8918.5118.7218.8018.4017.473CH 58.2857.7256.0757.8657.9658.2658.052CH COeth yl a cetat e21.0420.8320.6820.5621.1620.8821.153CO171.36170.96170.31170.44171.68172.89175.2660.4960.5659.7460.2160.9861.5062.32CH CH 214.1914.5014.4014.1914.5414.4913.923CH CO29.4929.3029.2628.5629.6029.3929.49ethyl m ethyl ketone3CO209.56208.30208.72206.55209.88212.16218.4336.8936.7535.8336.3637.0937.3437.27CH CH CH 2CH 37.868.037.617.918.148.097.8723CH ethylene glycol63.7964.2662.7664.3464.2264.3063.172CH “gr ease”29.7630.7329.2030.2130.8631.292CH n -hexane14.1414.3413.8814.3214.4314.453CH (2)22.7023.2822.0523.0423.4023.682CH (3)31.6432.3030.9531.9632.3632.732CH bH MP A36.8737.0436.4236.8837.1037.0036.463CH cmethanol50.4149.7748.5949.9749.9049.8649.503CH nitromethane62.5063.2163.2861.1663.6663.0863.223CH n -pentan e14.0814.2913.2814.2514.3714.393CH (2)22.3822.9821.7022.7223.0823.382CH (3)34.1634.8333.4834.4534.8935.302CH 2-propanol25.1425.6725.4325.1825.5525.2724.383CH64.5063.8564.9264.2364.3064.7164.88pyr idineCH (2)149.90150.67149.58150.27150.76150.07149.18CH (3)123.75124.57123.84123.58127.76125.53125.12CH (4)135.96136.56136.05135.28136.89138.35138.27silicon e gr ease1.041.401.382.10CH CH 3tetrahydrofuran25.6226.1525.1425.7226.2726.4825.672CH O67.9768.0767.0367.8068.3368.8368.682CH toluene21.4621.4620.9921.1021.5021.503C(i)137.89138.48137.35137.91138.90138.85CH (o)129.07129.76128.88129.33129.94129.91CH (m )128.26129.03128.18128.56129.23129.20CH (p)125.33126.12125.29125.68126.28126.29triethylamine11.6112.4911.7412.3512.3811.099.07CH CH 346.2547.0745.7446.7747.1046.9647.192
NMR 溶剂的化学位移为了方便讨论 , 贴出 NMR 溶剂的化学位移
NMR Solvents Solvent Formula 1H shifts 13C shifts <--mp °C bp °C --> mp °C bp °C
Acetic Acid-d4 CD3COOD 2.0, 11.7 20.0, 180.0 16.6 117.9
Acetone-d6 CD3COCD3 2.09 29.9, 206.7 -94.7 56.1
Acetonitrile-d3 CD3CN 1.94 1.4, 118.7 -43.8 81.6
Benzene-d6 C6D6 7.16 128.4 5.5 80.1
Carbon Disulphide CS2 none 192.8 -11.6 46.3
Carbon Tetrachloride CCl4 none 96.7 -23.0 76.8
Chloroform-d CDCl3 7.24 77.23 -63.5 61.3
Dichloromethane-d2 CD2Cl2 5.32 54.0 -95.1 40.8
Diethyl Ether (-100 °C) (CH3CH2)2O ?, 66.51 -116.3 34.6
Dimethyl Ether (-100 °C) CH3OCH3 3.2 60.08 -138.5 -23
N,N-Dimethyl formamide-d7 Me2NCHO 2.95, 2.75, 8.03 29.8, 34.9, 163.2 -61.? 153.?
Dimethyl Sulfoxide-d6 CD3SOCD3 2.50 39.5 18.6 189.0
1,4-Dioxan (OCH2CH2)2 3.53 66.7 11.8 101.4
Ethanol-d6 CD3CD2OD 1.11, 3.56, 5.19 17.3, 57.0 -117 78.3
Methanol-d4 CD3OD 3.31, 4.78 49.2 -97.8 64.6
Nitrobenzene C6D5NO2 7.5, 7.7, 8.1 123, 129, 135 5.7 210.8
Nitromethane-d3 CD3NO2 4.3 57.3 -28.6 101.2
Pyridine-d5 C5D5N 7.22, 7.58, 8.74 123.9, 135.9, 150.2 -41.6 115.3
1,1,2,2-Tetrachloroethane CHCl2CHCl2 ? 75.5 -43.8 146.3
Tetrahydrofuran-d8 C4D8O 1.73, 3.58 25.4, 67.6 -108.5 65.4
Tetrahydrofuran -100 °C C4H8O ?, 67.96
Toluene-d8 C6D5CD3 2.09, 6.98, 7.00, 7.09 20.4, 125.5, 128.3, 129.4, 137.9 -94.9 110.6
Trichlorofluoromethane CFCl3 none 117.6 -111 23.7
Trifluoroacetic Acid-d4 CF3COOD 11.5 116.6, 164.2 -15.3 72.4 Trifluoroethanol-d3 CF3CD2OD 3.88, 5.02 61.5, 126.3 -15.3 72.4 Water D2O 4.8 none 0.0 100.0
Solvent Formula 1H shifts 13C shifts <--mp °C bp °C --> mp °C bp °C
NMR溶剂的化学位移
作者:celan 文章来源:有机化学论坛 点击数:260 更新时间:2006-5-23
11.65 1 -- 178.99 1 -- Acetic Acid-d4 11.5 118 17 2.04 5 2.2 20.0 7 20
206.68 13 0.9 Acetone-d6 2.05 5 2.2 2.8 57 -94 29.92 7 19.4
118.69 1 -- Acetonitrile-d3 1.94 5 2.5 2.1 82 -45 1.39 7 21 Benzene-d6 7.16 1 -- 0.4 128.39 3 24.3 80 5 Chloroform-d 7.27 1 -- 1.5 77.23 3 32.0 62 -64 Cyclohexane-d12 1.38 1 -- -- 26.43 5 19 81 6 Deuterium Oxide 4.80 (DSS) 1 -- 4.8 -- -- -- 101.4 3.8
8.03 1 -- 163.15 3 29.4
N,N-Dimethyl-formamide 2.92 5 1.9 3.5 34.89 7 21.0 153 -61
2.75 5 1.9 29.76 7 21.1 Dimethyl Sulfoxide-d6 2.50 5 1.9 3.3 39.51 7 21.0 189 18 p-Dioxane-d6 3.53 m -- 2.4 66.66 5 21.9 101 12
5.29 1 -- -- -- Ethanol-d6 3.56 1 -- 5.3 56.96 5 22 79 <-130
1.11 m 17.31 7 19
4.87 1 -- -- -- -- Methanol-d4 4.9 65 -98 3.31 5 1.7 49.15 5 21.4 Methylene Chloride-d2 5.32 3 1.1 1.5 54.00 5 24.2 40 -95
8.74 1 150.35 3 27.5 Pyridine-d5 7.58 1 -- 5.0 135.91 3 24.5 116 -42
7.22 1 123.87 5 25
3.58 1 67.57 5 22.2 Tetrahydrofuran-d8 -- 2.4 - 2.5 66 -109 1.73 1 25.37 5 20.2
-- -- -- 137.86 1 --
7.09 m -- 129.24 3 23 Toluene-d8 7.00 1 -- 0.4 128.33 3 24 111 -95
6.98 m -- 125.49 3 24
2.09 5 2.3 20.4 7 19
164.2 4 Trifluoroacetic Acid-d 11.50 1 -- 11.5 72 -15 116.6 4
5.02 1 -- 126.3 4 -- Trifluoroethanol-d3 5 75 - 3.88 4x3 2 (9) 61.5 4x5 22
测试核磁的样品一般要求比较纯，并且能够溶解在氘代试剂中，这样才能测得高分辨率的图谱。 为不干扰谱图，所用溶剂分子中的氢都应被氘取代，但难免有氢的残余（1%左右），这样就会产生溶剂峰；除了残存的质子峰外，溶剂中有时会有微量的H2O 而产生水峰，而且这个H2O 峰的位置也会因溶剂的不同而不同；另外，在样品（或制备过程）中，也难免会残留一些杂质，在图谱上就会有杂质峰，应注意识别。
常用氘代溶剂和杂质峰在1H 谱中的化学位移 单位：ppm
溶剂 — CDCl3 (CD3)2CO (CD3)2SO C6D6 CD3CN CD3OH D2O
溶剂峰 — 7.26 2.05 2.49 7.16 1.94 3.31 4.80
水峰 — 1.56 2.84 3.33 0.40 2.13 4.87 —
乙酸 — 2.10 1.96 1.91 1.55 1.96 1.99 2.08
丙酮 — 2.17 2.09 2.09 1.55 2.08 2.15 2.22
乙腈 — 2.10 2.05 2.07 1.55 1.96 2.03 2.06
苯 — 7.36 7.36 7.37 7.15 7.37 7.33 —
叔丁醇CH3 1.28 1.18 1.11 1.05 1.16 1.40 1.24
OH — — 4.19 1.55 2.18 — —
叔丁基甲醚
CCH3 1.19 1.13 1.11 1.07 1.14 1.15 1.21
OCH3 3.22 3.13 3.08 3.04 3.13 3.20 3.22
氯仿 — 7.26 8.02 8.32 6.15 7.58 7.90 —
环己烷 — 1.43 1.43 1.40 1.40 1.44 1.45 —
1,2-二氯甲烷 3.73 3.87 3.90 2.90 3.81 3.78 —
二氯甲烷 — 5.30 5.63 5.76 4.27 5.44 5.49 —
乙醚 CH3(t) 1.21 1.11 1.09 1.11 1.12 1.18 1.17
CH2(q) 3.48 3.41 3.38 3.26 3.42 3.49 3.56
二甲基甲酰胺
CH 8.02 7.96 7.95 7.63 7.92 7.79 7.92
CH3 2.96 2.94 2.89 2.36 2.89 2.99 3.01 CH3 2.88 2.78 2.73 1.86 2.77 2.86 2.85 二甲基亚砜— 2.62 2.52 2.54 1.68 2.50 2.65 2.71
二氧杂环 — 3.71 3.59 3.57 3.35 3.60 3.66 3.75
乙醇 CH3(t) 1.25 1.12 1.06 0.96 1.12 1.19 1.17 CH2(q) 3.72 3.57 3.44 3.34 3.54 3.60 3.65 OH(s) 1.32 3.39 3.63 — 2.47 — — 乙酸乙酯CH3CO 2.05 1.97 1.99 1.65 1.97 2.01 2.07 OCH2(q) 4.12 4.05 4.03 3.89 4.06 4.09 4.14 CH3(t) 1.26 1.20 1.17 0.92 1.20 1.24 1.24 甲乙酮CH3CO 2.14 2.07 2.07 1.58 2.06 2.12 2.19 CH2(q) 2.46 2.45 2.43 1.81 2.43 2.50 3.18 CH3(t) 1.06 0.96 0.91 0.85 0.96 1.01 1.26 乙二醇 — 3.76 3.28 3.34 3.41 3.51 3.59 3.65 润滑脂 CH3(m) 0.86 0.87 — 0.92 0.86 0.88 — CH2(br) 1.26 1.29 — 1.36 1.27 1.29 — 正己烷CH3(t) 0.88 0.88 0.86 0.89 0.89 0.90 — CH2 (m) 1.26 1.28 1.25 1.24 1.28 1.29 — 甲醇 CH3 3.49 3.31 3.16 3.07 3.28 3.34 3.34 OH 1.09 3.12 4.01 2.16 — — 正戊烷 CH3(t) 0.88 0.88 0.86 0.87 0.89 0.90 — CH2(m) 1.27 1.27 1.27 1.23 1.29 1.29 — 异丙醇CH3(d) 1.22 1.10 1.04 0.95 1.09 1.50 1.17 CH 4.04 3.90 3.78 3.67 3.87 3.92 4.02 硅脂 — 0.07 0.13 — 0.29 0.08 0.10 — 四氢呋喃 CH2 1.85 1.79 1.76 1.40 1.80 1.87 1.88 CH2O 3.76 3.63 3.60 3.57 3.64 3.71 3.74 甲苯 CH3 2.36 2.32 2.30 2.11 2.33 2.32 — CH （o/p） 7.17 7.20 7.18 7.02 7.30 7.16 — CH （m ） 7.25 7.20 7.25 7.13 7.30 7.16 — 三乙基胺 CH3 1.03 0.96 0.93 0.96 0.96 1.05 0.99
CH2 2.53 2.45 2.43 2.40 2.45 2.58 2.57 石油醚 — 0.5-1.5 0.6-1.9 — — — — —
1常见溶剂的H在不同氘代溶剂中的化学位移值
氘 代 溶 剂 mult.
CDCl (CD)CO (CD)SO CD CDCN CDOD DO CDN 332326633255
7.20
残余溶剂峰 7.26 2.05 2.50 7.16 1.94 3.31 4.79 7.57
8.72
水峰 brs 1.56 2.84 3.33 0.40 2.13 4.87 4.79 4.96 s 7.26 8.02 8.32 6.15 7.58 7.90 CHCl 3
(CH)CO s 2.17 2.09 2.09 1.55 2.08 2.15 2.22 32
(CH)SO s 2.62 2.52 2.54 1.68 2.50 2.65 2.71 32
CH s 7.36 7.36 7.37 7.15 7.37 7.33 66
s 2.10 2.05 2.07 1.55 1.96 2.03 CHCN 2.06 3
CH,s 3.49 3.31 3.16 3.28 3 CHOH 3.07 3.34 3.34 3OH,s 1.09 3.12 4.01 2.16
CH(2),m 8.62 8.58 8.58 8.53 8.57 8.53 8.52 8.72 CH(3),m 7.29 7.35 7.39 6.66 7.33 7.44 7.45 7.20 CHN 55
CH(4),m 7.68 7.76 7.79 6.98 7.73 7.85 7.87 7.57
2.05 1.97 1.99 1.65 1.97 2.01 2.07 CH,s 3
4.12 4.05 4.03 3.89 4.06 4.09 4.14 CHCOOCH CH,q 3252
1.26 1.20 1.17 0.92 1.20 1.24 1.24 CH,t 3
CHCl s 5.30 5.63 5.76 4.27 5.44 5.49 22
0.88 0.88 0.86 0.89 0.89 0.90 CH,t 3n-hexane 1.26 1.28 1.25 1.24 1.28 1.29 CH,m 2
1.25 1.12 1.06 0.96 1.12 1.19 1.17 CH,t 3CHOH 253.72 3.57 3.44 3.34 3.54 3.60 3.65 CH,q 2
13常见溶剂的C在不同氘代溶剂中的化学位移值
氘 代 溶 剂
CDCl (CD)CO (CD)SO CD CDCN CDOD DO CDN 332326633255
123.44 206.26 1.32 溶剂峰 77.16 39.52 128.06 49.00 - 135.43 29.84 118.26 149.84 77.36 79.19 79.16 77.79 79.17 79.44 CHCl 3
207.07 205.87 206.31 204.43 207.43 209.67 215.94 30.92 30.60 30.56 30.14 30.91 30.67 30.89 (CH)CO 32
40.76 41.23 40.45 40.03 41.31 40.45 39.39 (CH)SO 32
128.37 129.15 128.30 128.62 129.32 129.34 CH 66
116.43 117.60 117.91 116.02 118.26 118.06 119.68 CHCN 31.89 1.12 1.03 0.20 1.79 0.85 1.47 50.41 49.77 48.59 49.97 49.90 49.86 49.50 CHOH 3
149.90 150.67 149.58 150.27 150.76 150.07 149.18 123.75 124.57 123.84 123.58 127.76 125.53 125.12 CHN 55
135.96 136.56 136.05 135.28 136.89 138.35 138.27 21.04 20.83 20.68 20.56 21.16 20.88 21.15 171.36 170.96 170.31 170.44 171.68 172.89 175.26 CHCOOCH 325 60.49 60.56 59.74 60.21 60.98 61.50 62.32 14.19 14.50 14.40 14.19 14.54 14.49 13.92
CHCl 53.52 54.95 54.84 53.46 55.32 54.78 22
14.14 14.34 13.88 14.32 14.43 14.45 n-hexane 22.70 23.28 22.05 23.04 23.40 23.68
31.64 32.30 30.95 31.96 32.36 32.73
18.41 18.89 18.51 18.72 18.80 18.40 17.47 CHOH 2558.28 57.72 56.07 57.86 57.96 58.26 58.05
*更多信息请参考"J.Org. Chem. 1997,62,7512-7515"