5-Bromo-2-nitropyridine was prepared
from the corresponding amine
via hydrogen peroxide oxidation in large scale production. This transformation
initially showed low conversion, high impurity content and lack of
reproducibility in lab trials. Parallel to process development, safety
studies were conducted to investigate the stability of oxidant mixture,
its composition and the oxidation reaction itself by reaction and
adiabatic calorimetry. The resulting robust reaction conditions and
appropriate safety boundaries allowed to develop a reproducible, safe
protocol for the implementation of this chemistry on large scale,
obtaining consistent results throughout the campaign.
In the course of a general programme aimed to find new protocols for environmentally friend chemistry [1-3] we were looking for a clean, high yielding method of reduction of 5-nitrosalicylic acid (1) to 5-aminosalicylic acid (5-ASA) in industrial scale [4].[...]
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