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An oscillatory plug flow photoreactor facilitates semi-heterogeneous dual nickel/carbon nitride photocatalytic C–N couplings
Reaction Chemistry & Engineering ( IF 3.9 ) Pub Date : 2020/02/14 , DOI: 10.1039/d0re00036a
Cristian Rosso 1, 2, 3, 4 , Sebastian Gisbertz 5, 6, 7, 8, 9 , Jason D. Williams 1, 2, 3, 4, 10 , Hannes P. L. Gemoets 11, 12, 13 , Wouter Debrouwer 12, 13, 14 , Bartholomäus Pieber 5, 6, 7, 8 , C. Oliver Kappe 1, 2, 3, 4, 10
Affiliation  

Carbon nitride materials have emerged as an efficient and sustainable class of heterogeneous photocatalysts, particularly when paired with nickel in dual catalytic cross-coupling reactions. Performing these transformations on larger scales using a continuous process is difficult due to the problems associated with handling solids in flow. By combining an oscillatory pump with a microstructured plug flow photoreactor, a stable suspension of the photocatalyst can be maintained, circumventing clogging of the reactor channels. Through careful tuning of the oscillator properties, the residence time distribution (RTD) was optimized, whilst maintaining a stable catalyst suspension. Short residence times (20 min) were achieved using optimized conditions and the recyclability of the photocatalyst was demonstrated over 10 cycles with no loss of activity. During a stable 4.5 hour scale-out demonstration, the model substrate could be isolated on 12 g scale (90% yield, 2.67 g h−1). Moreover, the method was applied for the gram scale synthesis of an intermediate of the active pharmaceutical ingredient tetracaine.

中文翻译:

振荡活塞流光反应器可促进半均相双镍/碳氮化物光催化C–N偶联

氮化碳材料已成为一种高效且可持续的多相光催化剂,特别是在双重催化交叉偶联反应中与镍配对时。由于与处理固体流有关的问题,使用连续过程在较大规模上进行这些转化是困难的。通过将振荡泵与微结构活塞流光反应器结合,可以保持光催化剂的稳定悬浮,从而避免了反应器通道的堵塞。通过仔细调整振荡器的性能,可以优化停留时间分布(RTD),同时保持稳定的催化剂悬浮液。使用优化的条件可以实现较短的停留时间(20分钟),并且在10个循环内证明了光催化剂的可回收性,且没有活性损失。-1)。此外,该方法被用于克级合成活性药物成分丁卡因的中间体。
更新日期:2020-03-03
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