Description:
<jats:p><jats:bold>Syntheses and Structure of Diborylacetylenes</jats:bold></jats:p><jats:p>Reactions of bis(trimethylstannyl)acetylene with 2‐chloro‐1,3,2‐benzodioxaborole derivatives or 9‐chloro‐9‐borabicyclo[3.3.1]nonane lead to the corresponding diborylacetylenes <jats:bold>1a, b</jats:bold> and <jats:bold>2</jats:bold>. Sodium acetylide reacts with R<jats:sup>1</jats:sup>R<jats:sup>2</jats:sup>BCl to give R<jats:sup>1</jats:sup>R<jats:sup>2</jats:sup>BC1 (<jats:bold>3a, b</jats:bold>), which are converted to R<jats:sup>1</jats:sup>R<jats:sup>2</jats:sup>BC1R<jats:sup>1</jats:sup>R<jats:sup>2</jats:sup> (<jats:bold>4a, b</jats:bold>) by lithiation and subsequent treatment with more R<jats:sup>1</jats:sup>R<jats:sup>2</jats:sup>BCl (R<jats:sup>1</jats:sup>=<jats:italic>i</jats:italic>Pr<jats:sub>2</jats:sub>N, R<jats:sup>2</jats:sup>=<jats:italic>i</jats:italic>Pr<jats:sub>2</jats:sub>N or <jats:italic>t</jats:italic>Bu). X‐Ray structure analyses are performed for <jats:bold>1a, 4a</jats:bold>, and <jats:bold>4b</jats:bold>.</jats:p>