Dissertation - Open Access
Master of Science (MS)
While sealed tube reactions have been used extensively in the synthesis of other transition metal complexes (1), the method has seen limited use in synthetic rhenium chemistry. The first reaction reported was the preparation of tris (l,1O phenanthroline) rhenium(III) chloride (2). The second reaction was an attempt to isomerize oxotrichlorobis (triphenylphosphine) rhenium(V), ReOCI3-[C65H5) 3P] 2; by refluxing it in chloroform (3). Instead of isomerization, oxodichloro(ethoxy) bis (triphenylphosphine) rhenium(V), ReO(OC2H5 )c12 [C65H5) 3P] was produced; the ethoxy moiety came from an ethanol preservative in commercial chloroform. As temperature was sometimes important, the isomerization was also attempted in chloroform.in a sealed tube at 120°c. The reaction unexpectedly gave compounds identified as tetrachlorobis( triphenylphosphine) rhenium(IV), ReCl4 -[C65H5) 3P]2, andtetrachlorobis (triphenylphosphineoxide) rhenium(IV), ReCl4 [C65H5) 3P]. The unusual behavior of the oxotrichlorobis (triphenylphosphine) rhenium(V) in the sealed tube led to the current work. The purpose of this project was to make a systematic investigation of sealed tube reactions of several rhenium co-ordination compounds in different solvents at variable temperatures. Complications arising in the recrystallization of one of the starting materials, oxotrichlorobis (triphenylphosphine) rheniurn(V), led to an investigation of a series of reactions producing triphenylphosphonium salts of several rhenium anions.
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South Dakota State University
Leitheiser, Melvin, "Reactions of Oxotrichlorobis(triphenylphosphine)rhenium(V)" (1969). Electronic Theses and Dissertations. 3556.