Synthesis
The Preparative Method of Di-t-Butyl Bromomalonate: by bromination of Malonic Acid with bromine in diethyl ether at rt followed by sulfuric acid catalyzed esterification with Isobutene in diethyl ether at rt; by bromination of di-t-butyl malonate with bromine and Calcium Carbonate in chloroform at rt followed by reflux; by lithiation of di-t-butyl malonate with n-Butyllithium in THF at -78 °C followed by addition of bromine and allowing reaction to warm to rt;10 by lithiation of di-t-butyl malonate with n-butyllithium in THF at -78 °C, addition of Chlorotrimethylsilane, warming to rt, and treatment of the resulting trimethylsilyl ketene acetal solution with bromine in carbon tetrachloride.
