Multikilogram per Hour Continuous Photochemical Benzylic Brominations Applying a Smart Dimensioning Scale-up Strategy,Organic Process Research & Development

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Multikilogram per Hour Continuous Photochemical Benzylic Brominations Applying a Smart Dimensioning Scale-up Strategy
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2020-06-15 , DOI: 10.1021/acs.oprd.0c00239
Alexander Steiner _{1,

2} , Philippe M. C. Roth ₃ , Franz J. Strauss ₄ , Guillaume Gauron ₃ , Günter Tekautz ₄ , Marc Winter ₃ , Jason D. Williams _{1,

2} , C. Oliver Kappe _{1,

2}

Affiliation

Although continuous flow technology can facilitate the scale-up of photochemical processes it is not yet routinely implemented on production scale in the fine chemical industries. This can be attributed to additional challenges compared to thermal processes, mostly in the homogeneous irradiation of the flow reactor. Here, we detail the process of bringing a previously developed photochemical benzylic bromination, utilizing in situ bromine generation, from lab to pilot scale. The process setup is discussed in detail, alongside a comprehensive risk assessment and discussion of problems encountered in the investigation of key reaction parameters. Ultimately, an assay yield of 88% was obtained in 22 s irradiated residence time, resulting in a productivity of 4.1 kg h^–1 (space-time yield = 82 kg L^–1 h^–1) representing a 14-fold scale-up versus the lab-scale process.

中文翻译：

每小时多千克的连续光化学苯甲酰溴应用智能尺寸放大策略

尽管连续流技术可以促进光化学工艺的规模化，但在精细化工行业中尚未在生产规模上常规实施。与热过程相比，这可以归因于额外的挑战，主要是在流动反应器的均匀辐照中。在这里，我们详细介绍了利用原位溴生成技术将先前开发的光化学苄基溴化技术从实验室规模扩大到中试规模的过程。除了详细的风险评估和关键反应参数研究中遇到的问题的讨论之外，还将详细讨论过程设置。最终，在22 s的辐照停留时间内，分析产率达到88％，生产率为4.1 kg h ^–1（时空产量= 82 kg L ^–1 h ^–1），相对于实验室规模的过程，规模扩大了14倍。

更新日期：2020-06-15

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