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2011•Chinese Journal of Energetic MaterialsRequires access

Improved Synthesis of 3,4-Dinitropyrazole

Fulei Gao

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Abstract

3,4-dinitropyrazole(DNP) was synthesized from pyrazole viaN-nitration,rearrangement andC-nitration.N-nitration was improved for a safe synthesis ofN-nitropyrazole and carried out by addition of pyrazole/acetic acid solution into nitric acid/acetic anhydride mixture.In addition,C-nitration conditions were optimized as follows:molar ratio of 3-nitropyrazole/nitric acid 1/2,nitration temperature 55-60℃,time 1 h.DNP′s total yield could be up to 55%,and purity 99%.The structures of the intermediate and the product were confirmed by IR,NMR,MS and element analysis.

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What this paper is about

3,4-dinitropyrazole(DNP) was synthesized from pyrazole viaN-nitration,rearrangement andC-nitration.N-nitration was improved for a safe synthesis ofN-nitropyrazole and carried out by addition of pyrazole/acetic acid solution into nitric acid/acetic anhydride mixture.In addition,C-nitration conditions were optimized as follows:molar ratio of 3-nitropyrazole/nitric acid 1/2,nitration temperature 55-60℃,time 1 h.DNP′s total yield could be up to 55%,and purity 99%.The structures of the intermediate and the product were confirmed by IR,NMR,MS and element analysis.

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Available abstract

3,4-dinitropyrazole(DNP) was synthesized from pyrazole viaN-nitration,rearrangement andC-nitration.N-nitration was improved for a safe synthesis ofN-nitropyrazole and carried out by addition of pyrazole/acetic acid solution into nitric acid/acetic anhydride mixture.In addition,C-nitration conditions were optimized as follows:molar ratio of 3-nitropyrazole/nitric acid 1/2,nitration temperature 55-60℃,time 1 h.DNP′s total yield could be up to 55%,and purity 99%.The structures of the intermediate and the product were confirmed by IR,NMR,MS and element analysis.

Key concepts: Nitration, Nitric acid, Acetic anhydride, Yield (engineering), Acetic acid, Chemistry, Molar ratio, Organic chemistry

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