N
X
C
Hal
O
N
S
P Si
Natural
Products
Solvents
C
C
C
C C
C
4.14 Spectra of Solvents and References
165
4.14.3 13 C NMR Spectrum of a Mixture of Common Nondeuterated
Solvents
The broad-band-decoupled 13 C NMR spectrum (125 MHz, δ in ppm relative to
TMS) of a CDCl 3 sample with 20 common solvents (0.05–0.4 vol%) shown below
serves as a guide to identify possible solvent impurities. Chemical shifts of signals
marked with an asterisk (*) may change up to a few ppm if the sample contains
solutes having functional groups that can form hydrogen bonds.
DMF: dimethyl formamide; THF: tetrahydrofuran; EGDME: ethylene glycol
dimethyl ether.
210 205 200 195 190 185 180 175 170 165 160 155 150 145 140
149.9* pyridine
DMF
162.5
ethyl acetate
171.1
192.6 CS 2
206.8* acetone
140 135 130 125 120 115 110 105 100 95 90 85 80 75
CDCl 3 77.1*
CHCl 3 77.3*
96.2* CCl 4
pyridine
136.0
128.4, 128.3 toluene, benzene
116.3* acetonitrile
125.3 toluene
129.1 toluene
toluene
137.9
123.8 pyridine
(top part
of signal
not
drawn)
75
70
65
60
55
50
methanol
50.7*
53.4 CH 2 Cl 2
59.1* ethanol
58.4 EGDME
67.1 dioxane
60.4 ethyl acetate
65.9 diethyl ether
THF 68.0
71.9 EGDME
50
45
40
35
30
25
25.6
THF
27.0 cyclohexane
DMF 36.4
30.9 acetone
DMF 31.3
hexane 31.6
dimethyl sulfoxide 41.1
25
20
15
10
5
0
TMS
1.8 acetonitrile
14.1 hexane
14.2 ethyl acetate
15.3 diethyl ether
18.5 ethanol
21.0 ethyl acetate
21.4 toluene
22.7 hexane
X
C
Hal
O
N
S
P Si
Natural
Products
Solvents
C
C
C
C C
C
4.14 Spectra of Solvents and References
165
4.14.3 13 C NMR Spectrum of a Mixture of Common Nondeuterated
Solvents
The broad-band-decoupled 13 C NMR spectrum (125 MHz, δ in ppm relative to
TMS) of a CDCl 3 sample with 20 common solvents (0.05–0.4 vol%) shown below
serves as a guide to identify possible solvent impurities. Chemical shifts of signals
marked with an asterisk (*) may change up to a few ppm if the sample contains
solutes having functional groups that can form hydrogen bonds.
DMF: dimethyl formamide; THF: tetrahydrofuran; EGDME: ethylene glycol
dimethyl ether.
210 205 200 195 190 185 180 175 170 165 160 155 150 145 140
149.9* pyridine
DMF
162.5
ethyl acetate
171.1
192.6 CS 2
206.8* acetone
140 135 130 125 120 115 110 105 100 95 90 85 80 75
CDCl 3 77.1*
CHCl 3 77.3*
96.2* CCl 4
pyridine
136.0
128.4, 128.3 toluene, benzene
116.3* acetonitrile
125.3 toluene
129.1 toluene
toluene
137.9
123.8 pyridine
(top part
of signal
not
drawn)
75
70
65
60
55
50
methanol
50.7*
53.4 CH 2 Cl 2
59.1* ethanol
58.4 EGDME
67.1 dioxane
60.4 ethyl acetate
65.9 diethyl ether
THF 68.0
71.9 EGDME
50
45
40
35
30
25
25.6
THF
27.0 cyclohexane
DMF 36.4
30.9 acetone
DMF 31.3
hexane 31.6
dimethyl sulfoxide 41.1
25
20
15
10
5
0
TMS
1.8 acetonitrile
14.1 hexane
14.2 ethyl acetate
15.3 diethyl ether
18.5 ethanol
21.0 ethyl acetate
21.4 toluene
22.7 hexane