A self optimizing synthetic organic reactor system using real-time in-line NMR spectroscopy

Abstract

A ‘dial-a-molecule’ platform for algorithm driven organic synthesis using real-time feedback, via in-line flow NMR spectroscopy, is demonstrated.

Advanced reactor engineering with 3D printing for the continuous-flow synthesis of silver nanoparticles

“…4 Asides the numerous benefits of heat transfer, mixing and kinetics, continuous flow reactors allow to characterise the product stream in-line with no disruption of the flow using spectroscopic techniques, thus allowing the real time monitoring, feedback and development of self-optimisation techniques. 5,6 Intensified reactors have found an ever increasing range of applications in synthetic chemistry from discovery 7,8 to the processing of high added value reactions including pharmaceuticals, 9 nanostructured 10 and advanced molecular materials. 3,11 In the microfluidic scale, the flow regime is laminar.…”

Online Monitoring of Polymerizations: Current Status

“…Duchateau and coworkers prepared Grignard reagents under continuous flow conditions with online NMR spectroscopy. [54] Cronin and coworkers [55] presented a platform for synthetic chemistry incorporating an inline benchtop NMR spectrometer that is capable of monitoring and controlling reactions in real-time as shown in Figure 4. Ley and coworkers [56] recently reported a setup for the continuous processing and in situ reaction monitoring of hypervalent iodine(III)-mediated cyclopropanation using benchtop NMR spectroscopy as shown in Figure 5.…”

Oxidative Neutralization of Mustard‐Gas Simulants in an On‐Board Flow Device with In‐Line NMR Monitoring

“…Actually,CEES proved to remain stable in aMSA/methanol mixture for hours in the absence of oxidant. [43] We incorporated such alow-field NMR system within our continuous flow system in order to evaluate the residence time t R at which the maximal conversion of CEES into the sulfoxyde CEESO is achieved (Figure 2). Neat CEES (23.36 mL, 0.2 mol), was pumped at af low rate of 0.5 mL min À1 and met in aT -shaped mixer as olution of UHP (1.3 equiv), MSA (2.6 equiv) in MeOH (30 equiv) pumped at af low rate of 5mLmin À1 .T he resulting stream entered in aP FA tubing reactor (ID = 1.6 mm, L = 10.7 m, V = 21.5 mL) with ar esidence time of t R = 3.9 minutes.T he reactor outlet was then collected into ab ottle containing 40 mL of 10 %( w/w) aqueous NaHSO 3 .T herefore,asimple extraction afforded the corresponding sulfoxide CEESO in > 99 %y ield.…”