Pairing Heterocyclic Cations with closo-Icosahedral Borane and Carborane Anions, II: Benchtop Alternative Synthetic Methodologies for Binary Triazolium and Tetrazolium Salts with Significant Water Solubility (POSTPRINT)
Abstract
Two efficient processes for the synthesis of twelve, relatively water soluble, heterocyclium closo-dodecaborane [B12H12]-2 and closo-dodecacarborane [CB11H12]-1 salts by a one-step, open-air metathesis reaction have been developed. First, a combination of exhaustive trituration of the two solid reactant salts with refluxing anhydrous acetonitrile followed by flash filtration through a plug of silica gel affords excellent recovery for a broad series of otherwise water-soluble salts. Second, an alternative aqueous metathesis, driven to completion by precipitation of silver halides, followed by removal of water, re-dissolution in acetonitrile, and filtration through a plug of silica gel, affords complex heterocyclium borane salts albeit with possible minor "bleed-through" of the by-product KNO3 salt. Mixed cation heterocyclium dodecaborane salts also can synthesized, and one example analyzed, shows melting point depression behavior.
Document Details
- Document Type
- Technical Report
- Publication Date
- Jan 01, 2012
- Accession Number
- ADA562467
Entities
People
- Brett A. Wight
- John L. Belletire
- Scott A. Shackelford
- Stefan Schneider
- Steven L. Strauss
Organizations
- Air Force Research Laboratory