An efficient two-stage method has been developed for the synthesis of perhalogenated monohydroxy derivatives of the -decaborate anion with the composition 2-BXOH (X = Cl, Br). The method involves complete halogenation of the boron framework in the initial DMF-containing derivative 2-BHOCHNMe by its reaction with sulfuryl chloride (SOCl) or elemental bromine (Br), followed by hydrolysis of the obtained perhalogenated derivatives 2-BXOCHNMe (X = Cl, Br) with hydrazine monohydrate (NH·HO). This synthetic approach allows for the production of the target compounds with high yield (80–85%) and high purity, as confirmed by a range of physicochemical analysis methods (multinuclear NMR spectroscopy on B, H, and C nuclei, IR spectroscopy, and elemental analysis). The structures of the 2-BXOCHNMe and 2-BXOH anions were determined by single-crystal X-ray diffraction analysis.
A.V. Golubev (Wed,) studied this question.
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