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A dual functionalization of 1,1‐diborylalkanes through deoxygenative enolization with carboxylic acids was developed. 1,1‐Diborylalkanes were activated by MeLi to generate α‐monoboryl carbanions. In situ IR spectroscopy indicated an interaction between carboxylic acid and 1,1‐diborylalkane before addition of the activation reagent. Release of the active α‐monoboryl carbanion from the masked form was...
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