Development of a Safe Continuous Process to Sodium Nitrotetrazolate via Solid Phase “Catch and Release”,Organic Process Research & Development

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Development of a Safe Continuous Process to Sodium Nitrotetrazolate via Solid Phase “Catch and Release”
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2021-07-14 , DOI: 10.1021/acs.oprd.1c00129
Robert H. Muir ₁ , Jon Bragg ₁ , Andrew Pearsall ₁ , Matthew Jorgensen ₁ , Brittany Sims ₁ , Kyle Yonoski ₁ , Neha Mehta ₂ , Jerry S. Salan ₁

Affiliation

Sodium nitrotetrazolate (NaNT) is a key intermediate to copper(I) nitrotetrazolate (DBX-1), a material of interest as a replacement for lead based primary explosives. Historical syntheses of NaNT were plagued with safety issues that prevented the large-scale manufacturing of NaNT. In this article, we detail the development of a safe process to generate NaNT in a continuous flow reactor via solid phase “catch and release”; a process that also reduces the formation of the most detrimental impurities that inhibit the synthesis of DBX-1. Furthermore, we discuss the demonstration of this process in 100 and 1000 mL continuous stirred tank reactors (CSTRs) and implications of scale-up of this process for robust production of NaNT at the manufacturing scale.

中文翻译：

通过固相“捕获和释放”开发硝基四唑钠的安全连续工艺

硝基四唑钠 (NaNT) 是硝基四唑酸铜 (I) (DBX-1) 的关键中间体，DBX-1 是一种令人感兴趣的材料，可替代铅基起爆药。NaNT 的历史合成受到安全问题的困扰，阻碍了 NaNT 的大规模制造。在本文中，我们详细介绍了通过固相“捕获和释放”在连续流动反应器中生成 NaNT 的安全工艺的开发；这一过程还可以减少抑制 DBX-1 合成的最有害杂质的形成。此外，我们讨论了该工艺在 100 和 1000 mL 连续搅拌釜反应器 (CSTR) 中的演示，以及该工艺的放大对以制造规模稳健生产 NaNT 的影响。

更新日期：2021-08-20

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