1H NMR CHEMICAL IMPURITY SHIFTS TABLE
proton mult CDCl3 (CD3)2CO (CD3)2SO C6D6 CD3CN CD3OD D2O
Solvent
residual
peak 7.26 2.05 2.50 7.16 1.94 3.31 4.79
H2O s 1.56 2.84 3.33 0.40 2.13 4.87
Acetic acid CH3 s 2.10 1.96 1.91 1.55 1.96 1.99 2.08
Acetone CH3 s 2.17 2.09 2.09 1.55 2.08 2.15 2.22
Acetonitrile CH3 s 2.10 2.05 2.07 1.55 1.96 2.03 2.06
Benzene CH s 7.36 7.36 7.37 7.15 7.37 7.33
Tert-butyl
alcohol CH3
OH s
s 1.28 1.18 1.11
4.19 1.05
1.55 1.16
2.18 1.40 1.24
Tert-butyl
methyl
ether CCH3
OCH3 s
s 1.19
3.22 1.13
3.13 1.11
3.08 1.07
3.04 1.14
3.13 1.15
3.20 1.21
3.22
BHTa ArH
OH
ArCH3 ArC(CH3)3 s
s
s
s 6.98 5.01 2.27 1.43 6.96
2.22
1.41 6.87
6.65
2.18
1.36 7.05 4.79 2.24 1.38 6.97
5.20
2.22
1.39 6.92
2.21
1.40
Chloroform CH s 7.26 8.02 8.32 6.15 7.58 7.90
Cyclohexane CH2 s 1.43 1.43 1.40 1.40 1.44 1.45
1,2-dichloro-
ethane CH2 s 3.73 3.87 3.90 2.90 3.81 3.78
Dichloro-
methane CH2 s 5.30 5.63 5.76 4.27 5.44 5.49
Diethyl ether CH3
CH2 t, 7
q, 7 1.21
3.48 1.11
3.41 1.09
3.38 1.11
3.26 1.12
3.42 1.18
3.49 1.17
3.56
Diglyme CH2
CH2
OCH3 m
m
s 3.65
3.57
3.39 3.56
3.47
3.28 3.51
3.38
3.24 3.46
3.34
3.11 3.53
3.45
3.29 3.61
3.58
3.35 3.67
3.61
3.37
1,2-dimeth-
oxyethane CH3
CH2 s
s 3.40
3.55 3.28
3.46 3.24
3.43 3.12
3.33 3.28
3.45 3.35
3.52 3.37
3.60
Dimethyl-
acetamide CH3CO
NCH3
NCH3 s
s
s 2.09
3.02
2.94 1.97
3.00
2.83 1.96
2.94
2.78 1.60
2.57
2.05 1.97
2.96
2.83 2.07
3.31
2.92 2.08
3.06
2.90
Dimethyl-
formamide CH
CH3
CH3 s
s
s 8.02
2.96
2.88 7.96
2.94
2.78 7.95
2.89
2.73 7.63
2.36
1.86 7.92
2.89
2.77 7.97
2.99
2.86 7.92
3.01
2.85
Dimethyl
sulfoxide CH3 s 2.62 2.52 2.54 1.68 2.50 2.65 2.71
Dioxane CH2 s 3.71 3.59 3.57 3.35 3.60 3.66 3.75
Ethanol CH3
CH2
OH t, 7
q, 7
s 1.25
3.72
1.32 1.12
3.57
3.39 1.06
3.44
4.63 0.96
3.34 1.12
3.54
2.47 1.19
3.60 1.17
3.65
Ethyl
acetate CH3CO
CH2CH3
CH2CH3 s
q, 7
t, 7 2.05
4.12
1.26 1.97
4.05
1.20 1.99
4.03
1.17 1.65
3.89
0.92 1.97
4.06
1.20 2.01
4.09
1.24 2.07
4.14
1.24
Ethyl methyl
ketone CH3CO
CH2CH3
CH2CH3 s
q, 7
t, 7 2.14
2.46
1.06 2.07
2.45
0.96 2.07
2.43
0.91 1.58
1.81
0.85 2.06
2.43
0.96 2.12
2.50
1.01 2.19
3.18
1.26
Ethylene
glycol CH s 3.76 3.28 3.34 3.41 3.51 3.59 3.65
“Grease” CH3
CH2 m
br s 0.86 1.26 0.87
1.29 0.92 1.36 0.86
1.27 0.88
1.29
N-hexane
CH3
CH2 t
m 0.88
1.26 0.88
1.28 0.86
1.25 0.89
1.24 0.89
1.28 0.90
1.29
HMPAb CH3 d,
9.5 2.65 2.59 2.53 2.40 2.57 2.64 2.61
Methanol CH3
OH s
s 3.49
1.09 3.31
3.12 3.16
4.01 3.07 3.28
2.16 3.34 3.34
Nitromethane CH3 s 4.33 4.43 4.42 2.94 4.31 4.34 4.40
n-pentane CH3
CH2 t, 7
m 0.88
1.27 0.88
1.27 0.86
1.27 0.87
1.23 0.89
1.29 0.90
1.29
2-propanol CH3
CH d, 6
sep,
6 1.22
4.04 1.10
3.90 1.04
3.78 0.95
3.67 1.09
3.87 1.50
3.92 1.17
4.02
Pyridine CH(2)
CH(3)
CH(4) m
m
m 8.62
7.29
7.68 8.58
7.35
7.76 8.58
7.39
7.79 8.53
6.66
6.98 8.57
7.33
7.73 8.53
7.44
7.85 8.52
7.45
7.87
Silicone grease CH3 s 0.07 0.13 0.29 0.08 0.10
Tetrahydro-
furan CH2
CH2O m
m 1.85
3.76 1.79
3.63 1.76
3.60 1.40
3.57 1.80
3.64 1.87
3.71 1.88
3.74
Toluene CH3
CH(o/p)
CH(m) s
m
m 2.36
7.17
7.25 2.32
7.1 – 7.2
7.1 – 7.2 2.30
7.18
7.25 2.11
7.02
7.13 2.33
7.1 – 7.3
7.1 – 7.3 2.32
7.16
7.16
Triethyl-
amine CH3
CH2 t, 7
q, 7 1.03
2.53 0.96
2.45 0.93
2.43 0.96
2.40 0.96
2.45 1.05
2.58 0.99
2.57
a 2,6-Dimethyl-4-tert-butylphenol
b Hexamethylphosophoramide
References
1.
Gottlieb HE, Kotlyar V, Nudelman A. 1997. J.Org.Chem., 62, 7512.
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