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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 271 records · Page 15
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DOE OSTI2023

Cost-efficient and Scalable Nitration of Cyanoacetic Acid with Potassium Nitrate in Methanesulfonic Acid Gives Pure 3,4-Dicyanofuroxan Following Modified Steam Distillation Methodologies

Two issues exist in the preparation of 3,4-dicyanofuroxan (1, DCFO) by a nitration of cyanoacetic acid (CAA) with 100% of HNO 3 in trifluoroacetic acid (TFA) or in H 2 SO 4 /CH 2 Cl 2 : (1) the cost of 100% of HNO 3 and (2) the isolation and purification of the product. In this paper, we report a cost-efficient nitration methodology by replacing 100% of HNO 3 with KNO 3 in methanesulfonic acid (MSA). The methodology includes adding KNO 3 and CAA portionwise to the solution of MSA at 45-50 ºC and keeping total nitrating time < 90 mins; purifying the product using our newly developed Water-Co-Distilling process or Modified Steam Distillation at atmosphere pressure. Here, the methodology, in general, provided DCFO in 50-60% of yield with >99% of purity as identified by NMR and GC-MS.

3,4-dicyanofuroxan↗