show their degree of variability.Occasionally,in order to distinguish between peaks who assignment was ambiguous,a further1-2µL of a specific substrate were added and the spectra run again.
Table1.1H NMR Data
proton mult CDCl3(CD3)2CO(CD3)2SO C6D6CD3CN CD3OD D2O solvent residual peak7.26 2.05 2.507.16 1.94 3.31 4.79 H2O s 1.56 2.84a 3.33a0.40 2.13 4.87
acetic acid CH3s 2.10 1.96 1.91 1.55 1.96 1.99 2.08 acetone CH3s 2.17 2.09 2.09 1.55 2.08 2.15 2.22 acetonitrile CH3s 2.10 2.05 2.07 1.55 1.96 2.03 2.06 benzene CH s7.367.367.377.157.377.33
tert-butyl alcohol CH3s 1.28 1.18 1.11 1.05 1.16 1.40 1.24 OH c s 4.19 1.55 2.18
tert-butyl methyl ether CCH3s 1.19 1.13 1.11 1.07 1.14 1.15 1.21 OCH3s 3.22 3.13 3.08 3.04 3.13 3.20 3.22 BHT b ArH s 6.98 6.96 6.877.05 6.97 6.92
OH c s 5.01 6.65 4.79 5.20
ArCH3s 2.27 2.22 2.18 2.24 2.22 2.21
ArC(CH3)3s 1.43 1.41 1.36 1.38 1.39 1.40
chloroform CH s7.268.028.32 6.157.587.90 cyclohexane CH2s 1.43 1.43 1.40 1.40 1.44 1.45
1,2-dichloroethane CH2s 3.73 3.87 3.90 2.90 3.81 3.78 dichloromethane CH2s 5.30 5.63 5.76 4.27 5.44 5.49
annoyingdiethyl ether CH3t,7 1.21 1.11 1.09 1.11 1.12 1.18 1.17 CH2q,7 3.48 3.41 3.38 3.26 3.42 3.49 3.56 diglyme CH2m 3.65 3.56 3.51 3.46 3.53 3.61 3.67 CH2m 3.57 3.47 3.38 3.34 3.45 3.58 3.61
OCH3s 3.39 3.28 3.24 3.11 3.29 3.35 3.37 1,2-dimethoxyethane CH3s 3.40 3.28 3.24 3.12 3.28 3.35 3.37 CH2s 3.55 3.46 3.43 3.33 3.45 3.52 3.60 dimethylacetamide CH3CO s 2.09 1.97 1.96 1.60 1.97 2.07 2.08 NCH3s 3.02 3.00 2.94 2.57 2.96 3.31 3.06
NCH3s 2.94 2.83 2.78 2.05 2.83 2.92 2.90 dimethylformamide CH s8.027.967.957.637.927.977.92 CH3s 2.96 2.94 2.89 2.36 2.89 2.99 3.01
CH3s 2.88 2.78 2.73 1.86 2.77 2.86 2.85 dimethyl sulfoxide CH3s 2.62 2.52 2.54 1.68 2.50 2.65 2.71 dioxane CH2s 3.71 3.59 3.57 3.35 3.60 3.66 3.75 ethanol CH3t,7 1.25 1.12 1.060.9
6 1.12 1.19 1.17 CH2q,7d 3.72 3.57 3.44 3.34 3.54 3.60 3.65
april是几月
OH s c,d 1.32 3.39 4.63 2.47
ethyl acetate CH3CO s 2.05 1.97 1.99 1.65 1.97 2.01 2.07
C H2CH3q,7 4.12 4.05 4.03 3.89 4.06 4.09 4.14
CH2C H3t,7 1.26 1.20 1.170.92 1.20 1.24 1.24 ethyl methyl ketone CH3CO s 2.14 2.07 2.07 1.58 2.06 2.12 2.19
C H2CH3q,7 2.46 2.45 2.43 1.81 2.43 2.50 3.18
CH2C H3t,7 1.060.960.910.850.96 1.01 1.26 ethylene glycol CH s e 3.76 3.28 3.34 3.41 3.51 3.59 3.65“grea”f CH3m0.860.870.920.860.88
CH2br s 1.26 1.29 1.36 1.27 1.29
n-hexane CH3t0.880.880.860.890.890.90中欧商学院mba
CH2m 1.26 1.28 1.25 1.24 1.28 1.29
handsome_boyHMPA g CH3d,9.5 2.65 2.59 2.53 2.40 2.57 2.64 2.61 methanol CH3s h 3.49 3.31 3.16 3.07 3.28 3.34 3.34 OH s c,h 1.09 3.12 4.01 2.16
nitromethane CH3s 4.33 4.43 4.42 2.94 4.31 4.34 4.40 n-pentane CH3t,70.880.880.860.870.890.90
CH2m 1.27 1.27 1.27 1.23 1.29 1.29
2-propanol CH3d,6 1.22 1.10 1.040.95 1.09 1.50 1.17 CH p,6 4.04 3.90 3.78 3.67 3.87 3.92 4.02 pyridine CH(2)m8.628.588.588.538.578.538.52 CH(3)m7.297.357.39 6.667.337.447.45
CH(4)m7.687.767.79 6.987.737.857.87 silicone grea i CH3s0.070.130.290.080.10 tetrahydrofuran CH2m 1.85 1.79 1.76 1.40 1.80 1.87 1.88 CH2O m 3.76 3.63 3.60 3.57 3.64 3.71 3.74 toluene CH3s 2.36 2.32 2.30 2.11 2.33 2.32
CH(o/p)m7.177.1-7.27.187.027.1-7.37.16
CH(m)m7.257.1-7.27.257.137.1-7.37.16 triethylamine CH3t,7 1.030.960.930.960.96 1.050.99 CH2q,7 2.53 2.45 2.43 2.40 2.45 2.58 2.57
找碴
a In the solvents the intermolecular rate of exchange is slow enough that a peak due to HDO is usually also obrved;it appears at
2.81and
3.30ppm in acetone and DMSO,respectively.In the former solvent,it is often en as a1:1:1triplet,with2J H,D)1Hz. b2,6-Dimethyl-4-tert-butylphenol.c The signals from exchangeable protons were not always identified.d In some cas(e note a),the coupling interaction between the CH2and the OH protons may be obrved(J)5Hz).e In CD3CN,the OH proton was en as a multiplet atδ2.69,and extra coupling was also apparent on the methylene peak.f Long-chain,linear aliphatic hydrocarbons.Their solubility in DMSO was too low to give visible peaks.g Hexamethylphosphoramide.h In some cas(e notes a,d),the coupling interaction between the CH3and the OH protons may be obrved(J)5.5Hz).i Poly(dimethylsiloxane).Its solubility in DMSO was too low to give visible peaks.
Notes J.Org.Chem.,Vol.62,No.21,19977513
pack it for me7514J.Org.Chem.,Vol.62,No.21,1997Notes
Table2.13C NMR Data a
property是什么意思
CDCl3(CD3)2CO(CD3)2SO C6D6CD3CN CD3OD D2O solvent signals77.16(0.0629.84(0.0139.52(0.06128.06(0.02 1.32(0.0249.00(0.01
206.26(0.13118.26(0.02
acetic acid CO175.99172.31171.93175.82173.21175.11177.21 CH320.8120.5120.9520.3720.7320.5621.03 acetone CO207.07205.87206.31204.43207.43209.67215.94 CH330.9230.6030.5630.1430.9130.6730.89 acetonitrile CN116.43117.60117.91116.02118.26118.06119.68 CH3 1.89 1.12 1.030.20 1.790.85 1.47 benzene CH128.37129.15128.30128.62129.32129.34
tert-butyl alcohol C69.1568.1366.8868.1968.7469.4070.36 CH331.2530.7230.3830.4730.6830.9130.29 tert-butyl methyl ether OCH349.4549.3548.7049.1949.5249.6649.37 C72.8772.8172.0472.4073.1774.3275.62
出国留学多少钱C C H326.9927.2426.7927.0927.2827.2226.60 BHT C(1)151.55152.51151.47152.05152.42152.85
C(2)135.87138.19139.12136.08138.13139.09
CH(3)125.55129.05127.97128.52129.61129.49
C(4)128.27126.03124.85125.83126.38126.11
CH3Ar21.2021.3120.9721.4021.2321.38
C H3C30.3331.6131.2531.3431.5031.15
C34.2535.0034.3334.3535.0535.36
chloroform CH77.3679.1979.1677.7979.1779.44
cyclohexane CH226.9427.5126.3327.2327.6327.96
1,2-dichloroethane CH243.5045.2545.0243.5945.5445.11 dichloromethane CH253.5254.9554.8453.4655.3254.78
diethyl ether CH315.2015.7815.1215.4615.6315.4614.77 CH265.9166.1262.0565.9466.3266.8866.42 diglyme CH359.0158.7757.9858.6658.9059.0658.67 CH270.5171.0369.5470.8770.9971.3370.05手续英语
CH271.9072.6371.2572.3572.6372.9271.63 1,2-dimethoxyethane CH359.0858.4558.0158.6858.895
9.0658.67 CH271.8472.4717.0772.2172.4772.7271.49 dimethylacetamide CH321.5321.5121.2921.1621.7621.3221.09 CO171.07170.61169.54169.95171.31173.32174.57postfix
NCH335.2834.8937.3834.6735.1735.5035.03
NCH338.1337.9234.4237.0338.2638.4338.76 dimethylformamide CH162.62162.79162.29162.13163.31164.73165.53 CH336.5036.1535.7335.2536.5736.8937.54
CH331.4531.0330.7330.7231.3231.6132.03 dimethyl sulfoxide CH340.7641.2340.4540.0341.3140.4539.39 dioxane CH267.1467.6066.3667.1667.7268.1167.19 ethanol CH318.4118.8918.5118.7218.8018.4017.47 CH258.2857.7256.0757.8657.9658.2658.05 ethyl acetate C H3CO21.0420.8320.6820.5621.1620.8821.15 CO171.36170.96170.31170.44171.68172.89175.26
CH260.4960.5659.7460.2160.9861.5062.32
CH314.1914.5014.4014.1914.5414.4913.92 ethyl methyl ketone C H3CO29.4929.3029.2628.5629.6029.3929.49 CO209.56208.30208.72206.55209.88212.16218.43
C H2CH336.8936.7535.8336.3637.0937.3437.27
CH2C H37.868.037.617.918.148.097.87 ethylene glycol CH263.7964.2662.7664.3464.2264.3063.17“grea”CH229.7630.7329.2030.2130.8631.29
n-hexane CH314.1414.3413.8814.3214.4314.45
CH2(2)22.7023.2822.0523.0423.4023.68
CH2(3)31.6432.3030.9531.9632.3632.73
HMPA b CH336.8737.0436.4236.8837.1037.0036.46 methanol CH350.4149.7748.5949.9749.9049.8649.50c nitromethane CH362.5063.2163.2861.1663.6663.0863.22 n-pentane CH314.0814.2913.2814.2514.3714.39
CH2(2)22.3822.9821.7022.7223.0823.38
CH2(3)34.1634.8333.4834.4534.8935.30
2-propanol CH325.1425.6725.4325.1825.5525.2724.38 CH64.5063.8564.9264.2364.3064.7164.88 pyridine CH(2)149.90150.67149.58150.27150.76150.07149.18 CH(3)123.75124.57123.84123.58127.76125.53125.12
CH(4)135.96136.56136.05135.28136.89138.35138.27 silicone grea CH3 1.04 1.40 1.38 2.10 tetrahydrofuran CH225.6226.1525.1425.7226.2726.4825.67 CH2O67.9768.0767.0367.8068.3368.8368.68 toluene CH321.4621.4620.9921.1021.5021.50
C(i)137.89138.48137.35137.91138.90138.85
CH(o)129.07129.76128.88129.33129.94129.91
CH(m)128.26129.03128.18128.56129.23129.20
CH(p)125.33126.12125.29125.68126.28126.29
triethylamine CH311.6112.4911.7412.3512.3811.099.07 CH246.2547.0745.7446.7747.1046.9647.19
a See footnotes for Table1.b2J PC)3Hz.c Reference material;e text.
