过氧化氢
化学
胺气处理
再现性
反应量热计
组合化学
量热法
有机化学
化学工程
色谱法
热力学
物理
工程类
作者
Alessandro Agosti,Giorgio Bertolini,Giacomo Bruno,Christian Lautz,Thomas Glarner,Walter Deichtmann
标识
DOI:10.1021/acs.oprd.6b00433
摘要
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.
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