Methods of preparing clusterboron

摘要

New methods are provided for synthesis of ClusterBoron® (B18H22). Preferred methods of the invention include generation of the conjugate acid of B20H182− and degradation of the acid in solution to produce B18H22 in high yields and high purity. The invention further provides isotopically enriched boranes, particularly isotopically enriched 10B18H22 and 11B18H22.

主权项

1. A method of synthesizing octadecaborane (B18H22), the method comprising:
(a) contacting the salt of borane anion B20H182− in a reaction solvent with an acid to produce a solution of H2B20H18●xH2O, wherein the reaction solvent is between about 80% and about 95% acetonitrile by volume; (b) concentrating the mixture comprising H2B20H18●xH2O; (c) removing water from the reaction vessel in the presence of a B18H22 solubilizing solvent that remains essentially chemically inert in the system, wherein the solubilizing solvent comprises an arene compound; and (d) separating insoluble byproducts from the reaction mixture through (i) filtration and/or (ii) concentration of reaction solvent, dissolution of B18H22 into a dissolution solvent and filtration of byproducts.