ICOSAHEDRAL CARBORANES. XIII. HALOGENATION OF P-CARBORANE

A method for the preparation and purification of substantial amounts of p-carborane is described. Chloro-, bromo- and iodo-p-carboranes were obtained via direct halogenation. The various halogenated species were separated by either column or vapor phase chromatography. In the chloro-p-carborane seri...

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Bibliographic Details
Main Authors: Sieckhaus,John F, Semenuk,Nick S, Knowles,Thomas A, Schroeder,Hansjuergen
Format: Report
Language:English
Subjects:
BORANES
BROMINE COMPOUNDS
CHLORINE COMPOUNDS
CHROMATOGRAPHIC ANALYSIS
ELECTROCHEMISTRY
HALOGENATION
Inorganic Chemistry
IODINE COMPOUNDS
MOLECULAR ISOMERISM
PHOTOCHEMICAL REACTIONS
PURIFICATION
STEREOCHEMISTRY
SYNTHESIS(CHEMISTRY)
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Summary:A method for the preparation and purification of substantial amounts of p-carborane is described. Chloro-, bromo- and iodo-p-carboranes were obtained via direct halogenation. The various halogenated species were separated by either column or vapor phase chromatography. In the chloro-p-carborane series, the mono-, nona- and decachlorinated compounds are individual species; the others occur as mixtures of geometrical isomers. Separation of the latter was accomplished by high resolution VPC using capillary column techniques. Interpretation of the chromatograms of these chlorinated derivatives proved consistent with the formation of all possible isomeric species in approximately those quantities which would be predicted on a statistical basis. None of these isomers was physically isolated, however. In contrast, partial fractionation of the dibromo- and diiodo-p-carborane isomer mixtures proved possible by common laboratory techniques. (Author)