Zhongyu Sun, Yuji Liu, Wei Huang, Ning Liu, Guangbin Cheng, Chuan Xiao* and Yongxing Tang*,
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Practical and Scalable Synthesis of 5,6-Dichlorofurazano[3,4-b]pyrazine
4H,8H-Difurazano[3,4-b:3′,4′-e]pyrazine (DFP) is an important heat-resistant explosive intermediate, but its current synthesis process is still not scalable due to the low yields and acidic smokes in an internal chlorination step to give the intermediate DHFP. In this work, a DMA-promoted chlorination method to synthesize 5,6-dichlorofurazano[3,4-b]pyrazine is described to solve the bottleneck of DFP synthesis. The best reaction conditions were confirmed to be DMA, DHFP, and POCl3 (2:1:40) at 120 °C for 3 h, with an increased yield of 62%. This new method not only increases the yield but also eliminates the acid smokes during postprocessing, and it is likely to find practical applications in the synthesis of DFP and other heat-resistant explosives.
期刊介绍：
The journal Organic Process Research & Development serves as a communication tool between industrial chemists and chemists working in universities and research institutes. As such, it reports original work from the broad field of industrial process chemistry but also presents academic results that are relevant, or potentially relevant, to industrial applications. Process chemistry is the science that enables the safe, environmentally benign and ultimately economical manufacturing of organic compounds that are required in larger amounts to help address the needs of society. Consequently, the Journal encompasses every aspect of organic chemistry, including all aspects of catalysis, synthetic methodology development and synthetic strategy exploration, but also includes aspects from analytical and solid-state chemistry and chemical engineering, such as work-up tools，process safety, or flow-chemistry. The goal of development and optimization of chemical reactions and processes is their transfer to a larger scale; original work describing such studies and the actual implementation on scale is highly relevant to the journal. However, studies on new developments from either industry, research institutes or academia that have not yet been demonstrated on scale, but where an industrial utility can be expected and where the study has addressed important prerequisites for a scale-up and has given confidence into the reliability and practicality of the chemistry, also serve the mission of OPR&D as a communication tool between the different contributors to the field.
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