|Fedick, Patrick Walter
The proposed research looks to develop and demonstrate a process to rapidly synthesize energetic materials through the utilization of non-traditional synthesis methodologies (i.e. confined volumes). Confined volume reactors, which encompass microdroplets, emulsions and thin films, etc. are synthetic methodologies that have shown accelerated product formation, by an order of 10 to 106, when compared to their counterpart traditional bulk reactions, (i.e. a round-bottom flask under reflux) depending on the reaction. The accelerated product formation of highly desired energetic compounds that customarily have lengthy, low-yield or cost-ineffective syntheses, such as synthetic steps in CL-20, will be targeted.The process of generating confined volume systems for accelerated synthesis of energetic materials and their precursors will be examined utilizing mass spectrometry ionization sources such as electrospray, nano-electrospray, paper spray, easy ambient sonic-spray, desorption electrospray, as well as, Leidenfrost droplets. The results from the accelerated synthesis of a known energetic syntheses, will be used as a guide for the exploration of alternative accelerated synthetic methods for prediction of other energetic materials and their precursory materials. Through the investigation of the fundamental phenomena that dictate the reaction mechanisms of alternative synthesis methodologies through confined volumes, these accelerated synthetic techniques can be leveraged to shorten the development of novel energetic materials and scale-up processes for milligram to gram quantities used for characterization. This proposal will seek to systematically answer the questions of what physical processes cause reactions to accelerate in confined volume systems and to what extent each process is responsible for acceleration to create desired products in the fastest and most effective manner possible while decreasing hazardous waste generated.
1.Patrick Fedick, Ryan Bain, Kinsey Bain, Tsdale Mehari, and R. Graham Cooks “Accelerated tert-Butyloxycarbonyl Deprotection of Amines in Microdroplets Produced by a Pneumatic Spray ” IJMS, (2018) DOI: 10.1016/j.ijms.2018.05.009
2. Xin Yan and R. Graham Cooks “Mass Spectrometry for Synthesis and Analysis ” Annual Review of Analytical Chemistry, (2018) DOI: 10.1146/annurev-anchem-061417-125820
3. Xin Yan, Ryan M. Bain, and R. Graham Cooks “Organic Reactions in Microdroplets: Reaction Acceleration Revealed by Mass Spectrometry”, Angew. Chem. Int. Ed., (2016) DOI: 10.1002/anie.201602270
Accelerated Reactions; Confined Volumes; Ambient Ionization; Mass Spectrometry; Energetics; Synthesis; High Throughput Screening