二次元NMR法によるシグナルの帰属

scopoletin

同様に C10H8O4の化合物 1mg/0.09ml acetone-d6の構造を推定せよ。ケミカルシフトの基準は溶媒の残留プロトン(δH 2.04 ppm)と溶媒のカーボンシグナル(δC 29.8 ppm)である。

1H-NMRスペクトル

1H-NMR spectrum of scopo acid

拡大

expansion of 1H-NMR spectrum of scopo acid

table

Peak List    Date: 11.08.2000    Time: 10:07
File Name:    f:\xwin_nmr\piccscop\1\pdata\1\1r
Peak Results saved in File:    -
Peak Picking Parameter:
Peak constant PC:    1.00
Noise:    0
Sens. level:    0
Peak Picking region:
Start(ppm)    Start(Hz)    End(ppm)    End(Hz)    MI(%)    MAXI(%)
14.05    7028.3    -2.07    -1036.2    -0.12    100.00
Peak Picking results:
Nr.   Point    Frequency    PPM    Intensity    %Int.
 1    10698    4395.41    8.7885      8317400     2.6
 2    12636    3918.45    7.8349     42097072    13.2
 3    12675    3908.85    7.8157     41635452    13.0
 4    13976    3588.66    7.1755     85629648    26.8
 5    14780    3390.79    6.7798     78642672    24.6
 6    16020    3085.62    6.1696     51825880    16.2
 7    16059    3076.02    6.1504     48094496    15.0
 8    20657    1944.41    3.8878    319926272   100.0
 9    22661    1451.20    2.9017     89909184    28.1
10    24394    1024.69    2.0489     27209056     8.5
11    24403    1022.48    2.0444     50090324    15.7
12    24412    1020.26    2.0400     69470352    21.7
13    24421    1018.05    2.0356     51650964    16.1
14    24429    1016.08    2.0316     28584216     8.9

13C-NMRスペクトル

13C COM and DEPT spectrum of scopo

table

Peak List    Date: 11.08.2000    Time:  9:48
File Name:    f:\xwin_nmr\piccscop\4\pdata\1\1R
Peak Results saved in File:    -
Peak Picking Parameter:
Peak constant PC:    1.00
Noise:    1087241
Sens. level:    4348965
Peak Picking region:
Start(ppm)    Start(Hz)    End(ppm)    End(Hz)    MI(%)    MAXI(%)
242.47    30492.2    -22.59    -2841.2    -1.45    100.00
Peak Picking results:
Nr.  Point    Frequency    PPM    Intensity    %Int.
 1     4480    25934.88    206.2290    274535168  100.0
 2    10036    20283.03    161.2866      5646853    2.1
 3    11205    19093.86    151.8306     10247584    3.7
 4    11295    19002.31    151.1026      8056893    2.9
 5    11932    18354.32    145.9499      7901324    2.9
 6    12096    18187.49    144.6233     24806428    9.0
 7    15973    14243.60    113.2623     25727162    9.4
 8    16122    14092.03    112.0570      7583542    2.8
 9    16383    13826.53    109.9458     18704006    6.8
10    17156    13040.19    103.6930     26407988    9.6
11    22967     7128.93     56.6879     23132900    8.4
12    26233     3806.59     30.2692     33086380   12.1
13    26252     3787.26     30.1155     91986912   33.5
14    26271     3767.93     29.9618    183316176   66.8
15    26290     3748.60     29.8082    210302704   76.6
16    26309     3729.28     29.6545    176347280   64.2
17    26328     3709.95     29.5008     86444376   31.5
18    26347     3690.62     29.3471     28621664   10.4

DEPT90
Peak List    Date: 11.08.2000    Time:  9:54
File Name:    f:\xwin_nmr\piccscop\2\pdata\1\1r
Peak Results saved in File:    -
Peak Picking Parameter:
Peak constant PC:    1.00
Noise:    13045397
Sens. level:    52181588
Peak Picking region:
Start(ppm)    Start(Hz)    End(ppm)    End(Hz)    MI(%)    MAXI(%)
242.47    30492.2    -22.59    -2841.2    -12.01    100.00
Peak Picking results:
Peak Nr.    Data Point    Frequency    PPM    Intensity    %Int.
 1    12096    18187.48    144.6232     245534864    61.9
 2    15973    14243.60    113.2622     270369568    68.2
 3    16384    13825.50    109.9377     396466240   100.0
 4    17156    13040.19    103.6930     325679360    82.1
DEPT135
Peak List    Date: 11.08.2000    Time:  9:54
File Name:    f:\xwin_nmr\piccscop\3\pdata\1\1r
Peak Results saved in File:    -
Peak Picking Parameter:
Peak constant PC:    1.00
Noise:    13045397
Sens. level:    52181588
Peak Picking region:
Start(ppm)    Start(Hz)    End(ppm)    End(Hz)    MI(%)    MAXI(%)
242.47    30492.2    -22.59    -2841.2    -12.46    100.00
Peak Picking results:
Peak Nr.    Data Point    Frequency    PPM    Intensity    %Int.
 1    12096    18187.48    144.6232     188873792    49.9
 2    15974    14242.58    113.2541     152104736    40.2
 3    16384    13825.50    109.9377     287420896    75.9
 4    17156    13040.19    103.6930     177830784    46.9
 5    22968     7127.91     56.6797     378809504   100.0

HSQC

HSQC spectrum of scopo

HMBC

HMBC spectrum of scopo Part of HMBC spectrum of scopo

NOE差スペクトル

NOE diffrence spectrum of scopo

化合物の構造


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