Application for fluorine compounds

  • Summary

NM200004E

ROYAL probe™ HFX can simultaneously irradiate 1H, 19F, and 13C (or other X-nuclei) even in a basic console with basic two-channel console, and is a versatile probe that can measure a wide-variety of nuclei at high sensitivity. Here we introduce some useful experiments for fluorine-containing compounds that can be run on conjunction with JNM-ECZ400S equipped with ROYALPROBE™ HFX.

Data 1: Triple-resonance measurement of 13C data.

13C signals of fluorinated compounds are typically split by the large JCF coupling. These splittings significantly decrease sensitivity and complicate data analysis . 13C{1H,19F} spectra can be most easily analyzed and another advantage is the full sensitivity as shown in Fig.1.

Data 2: 1H -19F HETCOR

1H-19F HETCOR(HETeronuclear CORrelation) is a very useful experiment for structure elucidation(Fig.2).

Fig. 1: Comparison of 13C, 13C{1H}, 13C{19F} and 13C{1H, 19F} spectra

Fig.1: Comparison of 13C, 13C{1H}, 13C{19F} and 13C{1H, 19F} spectra

  • Sample: 5% 1H,1H,2H,2H-perfluoro-1-octanol/CDCl3,
  • 13C: each 128 scans (exp. time = 7 min)
  • 1H-19F HETCOR: 2 scans (exp. time = 8 min)

CF3CF2CF2CF2CF2CF2CH2CH2OH

Fig. 2: 1H-19F HETCOR spectrum

Fig.2: 1H-19F HETCOR spectrum

Data 3: 1D 1H-19F HOESY

Trifluridine is a trifluoromethyl derivative of deoxyuridine that is used as an antineoplastic and antiviral agent. It is not easy to observe the correlation signal between 1H and 19F in this compound, since the 4-bond 1H-19F J-coupling is very small. 1D 1H-19F HOESY(Fig.3) is an effective method to selectively observe signal of protons which are spatially close to fluorine atoms within a couple of minutes. 2D 1H-19F HOESY can also provide similar information, but it takes several hours to collect 2D data. Fig.4 shows that the proton atom observed at 8.65 ppm is spatially close to the CF3 group.

Fig. 3: pulse sequence of 1D 1H-19F HOESY

Fig.3: pulse sequence of 1D 1H-19F HOESY

Fig. 4: 1D 1H-19F HOESY spectrum

Fig.4: 1D 1H-19F HOESY spectrum

Sample: 100mM Trifluridine in DMSO-d6
Upper spectrum: 1H, 8 scans (exp. time = 1 min),
Lower: HOESY, 16 scans (exp. time = 1 min),
mix_time = 1s

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