Carborane Synthesis.
Abstract
This report describes Phase I work done in thermolysis of tetraethylammonium borohydride (1-), (Et4NBH4) to tetraethylammonium decahydrodecaborate(2(-)), ((Et4N)2B10H10). The objective of this Phase I program was to solve the heat transfer requirements occurring during thermolysis. The nature of this requirement was to identify and optimize the reaction conditions of scale-up using boron and non-boron based solvents in the conversion of Et4NBH4 by thermolysis to (et4N)2B10H10. The critical steps in this requirement were to dissipate exothermic heat to minimize (Et4N)2B12H12 by-product formation and to maximize the desired (Et4N)2B10H10 product. Thermolysis of Et4NBH4, using triethylamine borane (Et3NBH3) as a boron-based solvent was demonstrated on a 50 g scale with (Et4N)2B10H10 yields up to 60%. Thermolysis of Et4NBH4 using mineral oil as the non-boron based solvent, demonstrated 47% yields.
Document Details
- Document Type
- Technical Report
- Publication Date
- Aug 28, 1979
- Accession Number
- ADA074570