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Author: Subject: New Klapötke patent for melt castable EM
Microtek
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[*] posted on 16-8-2023 at 12:58
New Klapötke patent for melt castable EM


So, as the title indicates, I recently stumbled on a patent by prof. Klapötke about bis(nitratoethyl)dinitroxamide which is produced by nitrating bis(hydroxyethyl)oxamide. This compound can be synthesized by reacting diethyloxalate with ethanolamine, and diethyloxalate is produced from ethanol and oxalic acid.
I made the diethyloxalate a few weeks ago, but did not have ethanolamine until recently. I have just tried the aminolysis of the ester, and it seems to proceed without issue. I did it in toluene as they write about in the patent, but I don't think that is necessary. Next step is nitration and purification.

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[*] posted on 21-8-2023 at 22:31


From another Klapötke paper, it seems that nitration with pure nitric acid leads to only O-nitration, ie. formation of nitric esters at the two OH groups. This produces another, significantly less dense and energetic material. It seems that nitration of the secondary amine moeities requires something more. In the patent they use oleum which could be prepared through one of the processes discussed here on SM. I think I will try N2O5 (via P2O5 and 100% HNO3) first, though. When I prepare oleum I get a lot of carbonization of stray organics, and it tends to make a mess unless I distill the oleum before use.
I think I will also do it as a two step nitration, first isolating the intermediate O-nitrated compound and then nitrating this further with N2O5 in nitric acid.

[Edited on 22-8-2023 by Microtek]
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[*] posted on 26-8-2023 at 13:14


Thanks
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