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

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6.1.2 Mass Spectrometry<br />

136<br />

Chapter Six<br />

Electron impact (EI) <strong>and</strong> fast atom bombardment (FAB) mass spectra were recorded on a<br />

Kratos concept 1H, double focussing forward geometry mass spectrometer. 3-Nitrobenzyl<br />

alcohol was used as <strong>the</strong> matrix for <strong>the</strong> FAB spectra. Electrospray mass spectra were<br />

obtained on a Micromass Quatro LC.<br />

6.1.3 Infrared Analysis<br />

Infra red spectra were recorded on a Perkin Elmer FT-IR spectrometer at 4 cm -1 resolution<br />

(16 scans) with a Universal ATR sampling accessory.<br />

6.1.4 Elemental Analysis<br />

All elemental analyses were performed by <strong>the</strong> Elemental Analysis Service at <strong>the</strong> London<br />

Metropolitan University.<br />

6.1.5 X-ray crystallography<br />

X-ray crystallography data were collected on a Bruker Apex SMART 2000 diffractometer.<br />

Crystal data <strong>and</strong> structure refinement can be found in <strong>the</strong> Appendix.<br />

6.1.6 Starting Materials<br />

Starting materials were used as received from Sigma Aldrich, Lancaster, Apollo,<br />

Fluorochem, ABCR, Alfa Aesar, Acros organics or Strem. Where dried solvents were<br />

necessary, dichloromethane, hexane, diethyl e<strong>the</strong>r, tetrahydr<strong>of</strong>uran, <strong>and</strong> acetonitrile were<br />

distilled using an Innovative Technology Pure Solv automated still. All dried solvents were<br />

stored in sealed ampoules under an atmosphere <strong>of</strong> dry nitrogen over 4Å molecular sieves.<br />

Pyridine was refluxed over calcium hydride <strong>and</strong> distilled into a dried ampoule under<br />

nitrogen.

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