Synthesis and Comparison of the Reactivity of Allyl Fluorides and ...

6.1 General Experimental Procedures
6 Experimental Details
6.1.1 Nuclear Magnetic Resonance Spectroscopy
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Chapter Six
The 1 H, 19 F{ 1 H}, 13 C{ 1 H} and 31 P{ 1 H} NMR spectra were recorded on a Bruker AM 300
spectrometer, a Bruker DRX 400 spectrometer or a Bruker AV 500 spectrometer at the
ambient temperature of the probe unless otherwise stated. 1 H and 13 C NMR spectra were
referenced internally using the residual protio solvent resonance relative to SiMe4 (δ = 0
ppm), whilst 19 F NMR were referenced to external CFCl3 (δ = 0 ppm) and 31 P NMR spectra
were referenced externally to 85 % H3PO4 (δ = 0 ppm). All chemical shifts are quoted in δ
(ppm) and coupling constants in Hertz (Hz), using the high-frequency positive convention.
Abbreviations have the usual meaning: s – singlet; d – doublet; t – triplet; q – quartet; qt –
quintet; ap - apparent. The following spectrometer frequencies were used:
Bruker AM 300 Spectrometer:
Bruker DRX 400 Spectrometer:
Bruker AV 500 Spectrometer:
1 H NMR spectra, 300.03 MHz,
13 C NMR spectra, 75.4426 MHz,
19 F NMR spectra, 282.3103 MHz,
31 P NMR spectra, 121.99 MHz.
1 H NMR spectra, 400.13 MHz,
13 C NMR spectra, 100.6128 MHz,
19 F NMR spectra, 376.4984 MHz,
31 P NMR spectra, 161.98 MHz.
1 H NMR spectra, 500.13 MHz,
13 C NMR spectra, 125.758 MHz.
The solvent most frequently used was deuterated chloroform (CDCl3) and data are reported
for samples dissolved in this solvent unless otherwise stated in the experimental data below.
However, if this was not possible due to solubility issues an alternative deutero solvent was
employed, and failing that a common laboratory solvent was used with a sealed, deuterated
benzene (C6D6), capillary insert tube. Spectra of air-/moisture-sensitive compounds were
obtained by preparing the samples under an inert atmosphere in a flush-box using dried
deuterated solvents. The solutions were then loaded into either a Young’s NMR tube or a
Teflon-sealed screw-cap NMR tube.