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Abstract <p>An efficient two-stage method has been developed for the synthesis of perhalogenated monohydroxy derivatives of the <i>closo</i>-decaborate anion with the composition [2-B<sub>10</sub>X<sub>9</sub>OH]<sup>2–</sup> (X = Cl, Br). The method involves complete halogenation of the boron cage in the initial DMF-containing derivative [2‑B<sub>10</sub>H<sub>9</sub>OCHNMe<sub>2</sub>]<sup>–</sup> by its reaction with sulfuryl chloride (SO<sub>2</sub>Cl<sub>2</sub>) or elemental bromine (Br<sub>2</sub>), followed by hydrolysis of the obtained perhalogenated derivatives [2-B<sub>10</sub>X<sub>9</sub>OCHNMe<sub>2</sub>]<sup>–</sup> (X = Cl, Br) with hydrazine monohydrate (N<sub>2</sub>H<sub>4</sub>·H<sub>2</sub>O). 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, including multinuclear <sup>11</sup>B, <sup>1</sup>H, and <sup>13</sup>C NMR spectroscopy, IR spectroscopy, and elemental analysis. The structures of the [2-B<sub>10</sub>X<sub>9</sub>OCHNMe<sub>2</sub>]<sup>–</sup> and [2-B<sub>10</sub>X<sub>9</sub>OH]<sup>2–</sup> anions were determined by single-crystal X-ray diffraction analysis.</p>

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Synthesis of Perhalogenated Monohydroxy Derivatives of the closo-Decaborate Anion [2-B10X9OH]2– (X = Cl, Br)

  • 期刊论文

  • 发表日期：

    2025年11月1日

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  • A. V. Golubev,
  • V. A. Mantsireva,
  • A. S. Kubasov,
  • A. Yu. Bykov,
  • K. Yu. Zhizhin,
  • N. T. Kuznetsov

摘要

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 cage 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, including multinuclear 11B, 1H, and 13C NMR spectroscopy, 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.