SYNTHESIS OF PERHALOGENATED MONOHYDROXY DERIVATIVES OF THE closo-DECABORATE ANION [2-B10X9OH]2– (X = Cl, Br)

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Abstract

An efficient two-stage method has been developed for the synthesis of perhalogenated monohydroxy derivatives of the closo-decaborate anion with the composition [2-B10X9OH]2– (X = Cl, Br). The method involves complete halogenation of the boron framework in the initial DMF-containing derivative [2-B10H9OCHNMe2]– by its reaction with sulfuryl chloride (SO2Cl2) or elemental bromine (Br2), followed by hydrolysis of the obtained perhalogenated derivatives [2-B10X9OCHNMe2]– (X = Cl, Br) with hydrazine monohydrate (N2H4·H2O). 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 11B, 1H, and 13C nuclei, IR spectroscopy, and elemental analysis). The structures of the [2-B10X9OCHNMe2]– and [2-B10X9OH]2– anions were determined by single-crystal X-ray diffraction analysis.

About the authors

A. V Golubev

N.S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Email: golalekseival@mail.ru
Moscow, Russia

V. A Mantsireva

N.S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences; D.I. Mendeleev University of Chemical Technology of Russia

Moscow, Russia

A. S Kubasov

N.S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Moscow, Russia

A. Yu Bykov

N.S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Moscow, Russia

K. Yu Zhizhin

N.S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Moscow, Russia

N. T Kuznetsov

N.S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Moscow, Russia

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