Synthesis and structure of 9-hydroxy-1,2-dicarba-closo-dodecaborane(11)

摘要

The oxidation of 1,2-C2B10H12 (1) with 100% nitric acid was studied in two solvents (CH(2)C1(2) and CCl4). Under the action of superacid (CF3SO3H), the compound 9-HO-1,2-C2B10H11 (2) gives the onium cation 9-H2O+-1,2-C2B10H11 involved in the salt [9-H2O+-1,2-C2B10Hn]-CF3SO3-, as demonstrated by B-u NMR spectroscopy. The experimental and simulated B-u NMR spectra of the cation 9-H2O+-1,2-C2B10H11 are in satisfactory agreement with each other. In the presence of a base, compound 2 is transferred from an ethereal solution to an aqueous alkaline solution giving the anion 9-O-- 1,2-C2B10H11. The structure of compound 2 was confirmed by H-1, B-11, (BH)-B-11-H-1, B-11-B-11 COSY NMR spectroscopy, IR spectroscopy, and gas chromatography mass spectrometry and was additionally established by X-ray diffraction.