Studying the Morita-Baylis-Hillman Reaction in Continuous Flow Using Packed Bed Reactors,Organic Process Research & Development

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Studying the Morita-Baylis-Hillman Reaction in Continuous Flow Using Packed Bed Reactors
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2018-10-17 00:00:00 , DOI: 10.1021/acs.oprd.8b00298
Rasmus A. T. Verdier ₁ , Jesper H. Mikkelsen ₁ , Anders T. Lindhardt ₁

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Conditions for the Morita-Baylis-Hillman reaction were developed under continuous flow using a packed bed reactor carrying 4-(dimethylamino)pyridine immobilized on silica. High reaction rates were obtained, as the packed bed reactor mimics super-stoichiometric catalyst loadings for the passing reaction mixture. Catalyst deactivation was circumvented by avoiding acrylate esters as the reaction partners. The developed flow protocol provided all desired Morita-Baylis-Hillman products in yields attaining 95% with typical retention times between just 30 and 60 min. Precise control of the retention time proved imperative for one example, in which optimal yield was attained in just 10 min, while outpacing sideproduct formation. Finally, a scale-out study was performed proving high stability of the packed bed reactor setup and catalyst for more than 20 h of operation.

中文翻译：

用填充床反应器研究连续流动中的森田-贝利斯-希尔曼反应

Morita-Baylis-Hillman反应的条件是使用载有固定在硅胶上的4-（二甲氨基）吡啶的填充床反应器在连续流动条件下开发的。由于填充床反应器模拟了通过的反应混合物的超化学计量催化剂负载，因此获得了高反应速率。通过避免丙烯酸酯作为反应伙伴来避免催化剂失活。开发的流程协议提供了所有所需的Morita-Baylis-Hillman产品，产率高达95％，典型保留时间仅为30至60分钟。一个实例证明了精确控制保留时间的必要性，其中仅在10分钟内即可达到最佳收率，同时超过了副产物的形成。最后，

更新日期：2018-10-17

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