Portland State University. Department of Chemistry.
Gary L. Gard
Date of Award
Master of Science (M.S.) in Chemistry
1 online resource (159 p.)
Sulphur pentafluoride, Fluorine compounds, Iodine compounds
Preparation of four SF5-containing fluoroalkyl iodides and derivatives thereof was accomplished beginning with a simplified synthesis of ICF2CF2I. Characterization of the products followed using a variety of spectroscopic and physical methods. The simplified method for preparing ICF2CF2I from iodine and tetrafluoroethylene (TFE) involved a reaction temperature of approximately 54°C and pressures of less than two atmospheres for the TFE. The synthesized ICF2CF2I was reacted with S2F1o and tetrafluoroethylene to give SF5CF2CF2I. The subsequent synthesis of the SFs containing fluoroalkyl iodides and derivatives were carried out using SFsCF2CF2I as the starting material in a Carius tube reaction vessel. The synthesized SFs containing compounds were: SFsCF2CF2CF2CF2I, SFsCF2CF2CH2CH20H, SFsCF2CF2CH2CHICH2CF=CF2, and SFsCF2CF2CH2CH2CH2CF=CF2. In addition, a derivative of the original starting material, ICF2CF2I, was prepared. This derivative was identified as ICH2CH2CF2CF2CH2CH2I. Techniques employed for the characterization of the products included infrared spectrometry, 13C, 19F and 1H nuclear magnetic resonance spectrometry, gas chromatography-mass spectrometry and elemental analysis. Melting point determinations were also performed for solid samples; boiling points were determined and used to characterize liquid samples.
Renn, Julia Anne, "Synthesis and Characterization of Novel SF5 Containing Fluoroalkyl Iodides and Derivatives" (1996). Dissertations and Theses. Paper 5309.