Thermolysis of tetraalkylammonium borohydrides to bis(tetraalkyl

Organic compounds -- part of the class 532-570 series – Organic compounds – Boron containing

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422130, 422202, 422205, 422225, 568 3, 568 5, C07F 502

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active

043919936

ABSTRACT:
Disclosed is an improved method and the thermolysis equipment setup for certing tetraethylammonium tetrahydridoborane to bis(tetraethylammonium) 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.degree. C. and 186.degree. 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 bis(tetraethylammonium) dodecahydrododecaborane while increasing the yield of the desired product, bis(tetraethylammonium) decahydrodecaborane.

REFERENCES:
patent: 2557910 (1951-06-01), Green
patent: 3313838 (1967-04-01), Rozzi
patent: 3525593 (1970-08-01), Thompson
patent: 4338289 (1982-07-01), Shore et al.

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