The
accessibility of bromonitromethane has declined in recent years,
limiting its viability as a reagent for chemical synthesis. The reinvestigation
and optimization of a variety of preparations, and the development
of safe operating principles, are described. The reproducible protocol
described here leverages the effectiveness of hydroxide for nitromethane
bromination while respecting its incompatibility with the product
it forms. This careful balance was achieved at scales up to 56 g,
resulting in a reproducible procedure that provides straightforward,
sustainable, and affordable access to this critical reagent.