Ammonium Dinitramide as a Prospective N–NO<sub>2</sub> Synthon: Electrochemical Synthesis of Nitro-<i>NNO</i>-Azoxy Compounds from Nitrosoarenes

In this study, the electrochemical coupling of nitrosoarenes with ammonium dinitramide is discovered, leading to the facile construction of the nitro-<i>NNO</i>-azoxy group, which represents an important motif in the design of energetic materials. Compared to known approaches to nitro-&l...

Full description

Saved in:
Bibliographic Details
Main Authors: Alexander S. Budnikov, Nikita E. Leonov, Michael S. Klenov, Mikhail I. Shevchenko, Tatiana Y. Dvinyaninova, Igor B. Krylov, Aleksandr M. Churakov, Ivan V. Fedyanin, Vladimir A. Tartakovsky, Alexander O. Terent’ev
Format: Article
Language:English
Published: MDPI AG 2024-11-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/29/23/5563
Tags: Add Tag
No Tags, Be the first to tag this record!
_version_ 1850260414817894400
author Alexander S. Budnikov
Nikita E. Leonov
Michael S. Klenov
Mikhail I. Shevchenko
Tatiana Y. Dvinyaninova
Igor B. Krylov
Aleksandr M. Churakov
Ivan V. Fedyanin
Vladimir A. Tartakovsky
Alexander O. Terent’ev
author_facet Alexander S. Budnikov
Nikita E. Leonov
Michael S. Klenov
Mikhail I. Shevchenko
Tatiana Y. Dvinyaninova
Igor B. Krylov
Aleksandr M. Churakov
Ivan V. Fedyanin
Vladimir A. Tartakovsky
Alexander O. Terent’ev
author_sort Alexander S. Budnikov
collection DOAJ
description In this study, the electrochemical coupling of nitrosoarenes with ammonium dinitramide is discovered, leading to the facile construction of the nitro-<i>NNO</i>-azoxy group, which represents an important motif in the design of energetic materials. Compared to known approaches to nitro-<i>NNO</i>-azoxy compounds involving two chemical steps (formation of azoxy group containing a leaving group and its nitration) and demanding expensive, corrosive, and hygroscopic nitronium salts, the presented electrochemical method consists of a single step and is based solely on nitrosoarenes and ammonium dinitramide. The dinitramide salt plays the roles of both the electrolyte and reactant for the coupling. Despite the fact that many side reactions can be expected due to the redox-activity of both the reagents and target products, under optimized conditions the synthesis is performed in an undivided cell under constant current conditions with high current density and can be easily scaled up without a reduction in the product yield. Moreover, the synthesized nitro-<i>NNO</i>-azoxy compounds are discovered to be potent fungicides active against a broad range of phytopathogenic fungi.
format Article
id doaj-art-fb17c9ef728643a2aa63d7cd3834e4f7
institution OA Journals
issn 1420-3049
language English
publishDate 2024-11-01
publisher MDPI AG
record_format Article
series Molecules
spelling doaj-art-fb17c9ef728643a2aa63d7cd3834e4f72025-08-20T01:55:38ZengMDPI AGMolecules1420-30492024-11-012923556310.3390/molecules29235563Ammonium Dinitramide as a Prospective N–NO<sub>2</sub> Synthon: Electrochemical Synthesis of Nitro-<i>NNO</i>-Azoxy Compounds from NitrosoarenesAlexander S. Budnikov0Nikita E. Leonov1Michael S. Klenov2Mikhail I. Shevchenko3Tatiana Y. Dvinyaninova4Igor B. Krylov5Aleksandr M. Churakov6Ivan V. Fedyanin7Vladimir A. Tartakovsky8Alexander O. Terent’ev9N. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prosp., 119991 Moscow, RussiaN. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prosp., 119991 Moscow, RussiaN. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prosp., 119991 Moscow, RussiaN. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prosp., 119991 Moscow, RussiaN. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prosp., 119991 Moscow, RussiaN. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prosp., 119991 Moscow, RussiaN. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prosp., 119991 Moscow, RussiaA. N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilova Str., 119991 Moscow, RussiaN. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prosp., 119991 Moscow, RussiaN. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prosp., 119991 Moscow, RussiaIn this study, the electrochemical coupling of nitrosoarenes with ammonium dinitramide is discovered, leading to the facile construction of the nitro-<i>NNO</i>-azoxy group, which represents an important motif in the design of energetic materials. Compared to known approaches to nitro-<i>NNO</i>-azoxy compounds involving two chemical steps (formation of azoxy group containing a leaving group and its nitration) and demanding expensive, corrosive, and hygroscopic nitronium salts, the presented electrochemical method consists of a single step and is based solely on nitrosoarenes and ammonium dinitramide. The dinitramide salt plays the roles of both the electrolyte and reactant for the coupling. Despite the fact that many side reactions can be expected due to the redox-activity of both the reagents and target products, under optimized conditions the synthesis is performed in an undivided cell under constant current conditions with high current density and can be easily scaled up without a reduction in the product yield. Moreover, the synthesized nitro-<i>NNO</i>-azoxy compounds are discovered to be potent fungicides active against a broad range of phytopathogenic fungi.https://www.mdpi.com/1420-3049/29/23/5563electrochemistryN–N couplingazoxy compoundsammonium dinitramidenitroso compoundsantifungal agents
spellingShingle Alexander S. Budnikov
Nikita E. Leonov
Michael S. Klenov
Mikhail I. Shevchenko
Tatiana Y. Dvinyaninova
Igor B. Krylov
Aleksandr M. Churakov
Ivan V. Fedyanin
Vladimir A. Tartakovsky
Alexander O. Terent’ev
Ammonium Dinitramide as a Prospective N–NO<sub>2</sub> Synthon: Electrochemical Synthesis of Nitro-<i>NNO</i>-Azoxy Compounds from Nitrosoarenes
Molecules
electrochemistry
N–N coupling
azoxy compounds
ammonium dinitramide
nitroso compounds
antifungal agents
title Ammonium Dinitramide as a Prospective N–NO<sub>2</sub> Synthon: Electrochemical Synthesis of Nitro-<i>NNO</i>-Azoxy Compounds from Nitrosoarenes
title_full Ammonium Dinitramide as a Prospective N–NO<sub>2</sub> Synthon: Electrochemical Synthesis of Nitro-<i>NNO</i>-Azoxy Compounds from Nitrosoarenes
title_fullStr Ammonium Dinitramide as a Prospective N–NO<sub>2</sub> Synthon: Electrochemical Synthesis of Nitro-<i>NNO</i>-Azoxy Compounds from Nitrosoarenes
title_full_unstemmed Ammonium Dinitramide as a Prospective N–NO<sub>2</sub> Synthon: Electrochemical Synthesis of Nitro-<i>NNO</i>-Azoxy Compounds from Nitrosoarenes
title_short Ammonium Dinitramide as a Prospective N–NO<sub>2</sub> Synthon: Electrochemical Synthesis of Nitro-<i>NNO</i>-Azoxy Compounds from Nitrosoarenes
title_sort ammonium dinitramide as a prospective n no sub 2 sub synthon electrochemical synthesis of nitro i nno i azoxy compounds from nitrosoarenes
topic electrochemistry
N–N coupling
azoxy compounds
ammonium dinitramide
nitroso compounds
antifungal agents
url https://www.mdpi.com/1420-3049/29/23/5563
work_keys_str_mv AT alexandersbudnikov ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes
AT nikitaeleonov ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes
AT michaelsklenov ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes
AT mikhailishevchenko ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes
AT tatianaydvinyaninova ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes
AT igorbkrylov ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes
AT aleksandrmchurakov ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes
AT ivanvfedyanin ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes
AT vladimiratartakovsky ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes
AT alexanderoterentev ammoniumdinitramideasaprospectivennosub2subsynthonelectrochemicalsynthesisofnitroinnoiazoxycompoundsfromnitrosoarenes