| Summary: | A green, fast and selective approach for the synthesis of mono-substituted <i>closo</i>-decaborate derivatives [2-B<sub>10</sub>H<sub>9</sub>COR]<sup>2−</sup> has been established via a nucleophilic addition reaction between the carbonyl derivative of <i>closo</i>-decaborate [2-B<sub>10</sub>H<sub>9</sub>CO]<sup>−</sup> and the corresponding Grignard reagent RMgX, where R is the ethyl, iso-propyl, pentyl, allyl, vinyl and propynyl groups. This approach is accomplished under mild conditions with 70–80% yields. The significance of these derivative is their ability to constitute building blocks for polymeric integration via the allyl, vinyl and propynyl substituents. All products were characterized by <sup>11</sup>B, <sup>1</sup>H and <sup>13</sup>C NMR, elemental analysis and mass spectrometry.
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