This paper describes a flow chemistry approach for synthesising two high-energy molecules, cyanuric triazide (CTA) and 2,4-dinitroanisole (DNAN), and scaling them up to multi-gram scale using an automated flow reactor system. The flow chemistry approach offers high degree of safety and easy to scale compared to conventional syntheses. The development of two processes: a. CTA via azidation of cyanuric chloride; b. DNAN via methoxylation of 2,4-dinitri-chlorobenzene (2,4-DNCB) on an automated commercially available flow reactor system is described. High yield (> 95%) was achieved in both the processes. Very short reaction times (30 seconds) were applied. The process parameters were optimized using the automated flow chemistry system. The optimized process was scaled to multi gram scale (> 30 g/hr). The method can be considered fit for the safe production of CTA and DNAN at multi gram scale in laboratory.
This paper describes a safer, scalable and continuous process for synthesis of picramide. The process consists of two steps: step-1. nitration of p-nitroanisole (PNAN) to 2,4,6-trinitrianisole (TNAN); step-2. ammonolysis of TNAN to picramide. Both the steps were optimized in flow, with yield of 90% and 98% in step-1 and step-2 respectively. Picramide with HPLC purity greater than 99% was obtained. When compared with batch, in step-1, flow process provided significant advantage in selectivity and yield. The optimized flow process was scaled to 25 g/hr production rate in a laboratory flow reactor. The method can be considered fit for the safe production of picramide at commercial scale.
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