Perylene
dyes are a cornerstone of modern research and technology
in fields ranging from printed (opto)electronics to bioimaging. Most
known compounds are bisimide derivatives prepared from perylenetetracarboxylic
dianhydride (PTCDA), which is essentially a chemical commodity. On
the contrary, there are comparatively fewer reports on perylenedicarboxylic
monoimide derivatives not due to lack of performance but due to the
challenging access to the key intermediate 3,4-perylenedicarboxylic
monoanhydride (PDCMA). As we detail, reported synthetic pathways are
both costly, resource intensive, and associated with extremely poor
green metrics. We show a new two-step straightforward, sustainable,
efficient, and organic solvent-free preparation of PDCMA based on
a combination of solventless and in-water reactions.