Thermolysis of Tetraalkylammonium Borohydrides to Bis(tetraalkylammonium) Decahydrodecaboranes.
DEPARTMENT OF THE ARMY WASHINGTON DC
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Disclosed is an improved method and the thermolysis equipment setup for converting tetraethylammonium tetrahydridoborane to bistetraethylammonium decahydrodecaborane by a thermolysis reaction which increases the yield in the range between about 22 to 64, and, perhaps higher. The heat transfer control is maintained by employing triethylamine borane in the reaction mixture between about 175 degrees C. and 186 degrees C. for a reaction time from about 1 hour to about 2.5 hours. The disclosed thermolysis procedure is successful in dissipating a major portion of the exothermic heat. The control of the generated heat serves to minimize the formation of the byproduct bistetraethylammonium dodecahydrododecaborane while increasing the yield of the desired product, bistetraethylammonium decahydrodecaborane. Author
- Organic Chemistry