Diethyl furoxan dicarboxylate (DFD) is a starting material for fields as diverse as drug discovery, energetics, and any application where a furoxan or furazan may be desired. As with many disubstituted furoxans, they are synthesized via the dimerization of the appropriate nitrile oxide. Past procedures to form DFD involve low-yield destructive nitrations, multiple steps, halogenated solvents, or heavy or precious metals. Although these methods are functional enough for lab-scale preparations of DFD, they do not hold up well for economical scale-up. Our reported procedure improves the synthesis of DFD such that it is available from economical and commercially available starting materials in a single-step, one-pot, high-yield (98.5%) synthesis of material with a trivial workup in high purity (98.2% by ¹H quantitative NMR against a 2,4,6-trimethoxy-1,3,5-triazene standard). This improved procedure requires no organic solvents or heavy metals and is the most scalable preparation for this material to date.

中文翻译：

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经济、一锅法合成呋喃生二羧酸二乙酯


呋喃喃二乙酯二羧酸酯 （DFD） 是药物发现、能量学以及任何可能需要呋喃喃或呋喃散的应用等不同领域的起始材料。与许多二取代呋喃烷一样，它们是通过适当的腈氧化物二聚化合成的。过去形成 DFD 的程序涉及低产率的破坏性硝化、多个步骤、卤化溶剂或重金属或贵金属。尽管这些方法对于实验室规模的 DFD 制备功能足够，但它们不能很好地实现经济的放大。我们报道的程序改进了 DFD 的合成，使其可以从经济和市售的起始材料中获得，以一步、一瓶、高产率 （98.5%） 合成材料，只需简单的高纯度处理^{（1 小时}定量 NMR 对 2,4,6-三甲氧基-1,3,5-三氮嗪标准品的定量 NMR 为 98.2%）。这种改进的程序不需要有机溶剂或重金属，是迄今为止针对这种材料最具可扩展性的制剂。