Nucleophilic Addition Reactions to 10-Acetonitrilium Derivative of <i>nido</i>-Carborane and Intramolecular NH⋯HB Interactions in <i>N</i>-Alkyl Amidines 10-RNHC(Me)=NH-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>

The addition reactions of water, alcohols, and primary and secondary amines to the 10-acetonitrilium derivative of <i>nido</i>-carborane were studied. Hydrolysis of 10-MeC≡N-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> results in iminol 10-MeC(OH)=HN-7...

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Main Authors: Kirill R. Pakholkov, Ekaterina V. Bogdanova, Marina Yu. Stogniy, Kyrill Yu. Suponitsky, Sergey A. Anufriev, Igor B. Sivaev, Vladimir I. Bregadze
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Language:English
Published: MDPI AG 2025-02-01
Series:Molecules
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Online Access:https://www.mdpi.com/1420-3049/30/4/828
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author Kirill R. Pakholkov
Ekaterina V. Bogdanova
Marina Yu. Stogniy
Kyrill Yu. Suponitsky
Sergey A. Anufriev
Igor B. Sivaev
Vladimir I. Bregadze
author_facet Kirill R. Pakholkov
Ekaterina V. Bogdanova
Marina Yu. Stogniy
Kyrill Yu. Suponitsky
Sergey A. Anufriev
Igor B. Sivaev
Vladimir I. Bregadze
author_sort Kirill R. Pakholkov
collection DOAJ
description The addition reactions of water, alcohols, and primary and secondary amines to the 10-acetonitrilium derivative of <i>nido</i>-carborane were studied. Hydrolysis of 10-MeC≡N-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> results in iminol 10-MeC(OH)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>, which, on treatment with a base, gives amide [10-MeC(=O)HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>]<sup>−</sup>. The reactions of 10-MeC≡N-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> with alcohols lead to imidates 10-ROC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> (R = Me, Et) as mixtures of <i>E</i>- and <i>Z</i>-isomers. In the solid state, 10-MeOC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> adopts <i>E</i>-configuration. The reactions of 10-MeC≡N-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> with primary amines result in amidines 10-RNHC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> (R = Me, Et) as mixtures of <i>E</i>- and <i>Z</i>-isomers. In the solid state 10-EtNHC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> was found to have the <i>Z</i>-configuration, which is stabilized by intramolecular N-H⋯H-B interactions between the NH group originating from the primary amine and the BH group of the carborane cage. These interactions are rather strong (3.7 kcal/mol) and are likely to persist in solution. The reactions of 10-MeC≡N-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> with secondary acyclic (Me<sub>2</sub>NH, Et<sub>2</sub>NH) and cyclic (piperidine, morpholine) amines result in amidines 10-R<sub>2</sub>NC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> (R = Me, Et; R<sub>2</sub> = N(CH<sub>2</sub>)<sub>5</sub>, N(CH<sub>2</sub>CH<sub>2</sub>)<sub>2</sub>O) as single isomers, which, according to single crystal X-ray diffraction data, have the <i>E</i>-configuration.
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spelling doaj-art-7a887ce5c13b4ecbb144f9a36dbc6c912025-08-20T03:12:09ZengMDPI AGMolecules1420-30492025-02-0130482810.3390/molecules30040828Nucleophilic Addition Reactions to 10-Acetonitrilium Derivative of <i>nido</i>-Carborane and Intramolecular NH⋯HB Interactions in <i>N</i>-Alkyl Amidines 10-RNHC(Me)=NH-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>Kirill R. Pakholkov0Ekaterina V. Bogdanova1Marina Yu. Stogniy2Kyrill Yu. Suponitsky3Sergey A. Anufriev4Igor B. Sivaev5Vladimir I. Bregadze6A.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilov Str., 119991 Moscow, RussiaA.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilov Str., 119991 Moscow, RussiaA.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilov Str., 119991 Moscow, RussiaA.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilov Str., 119991 Moscow, RussiaA.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilov Str., 119991 Moscow, RussiaA.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilov Str., 119991 Moscow, RussiaA.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilov Str., 119991 Moscow, RussiaThe addition reactions of water, alcohols, and primary and secondary amines to the 10-acetonitrilium derivative of <i>nido</i>-carborane were studied. Hydrolysis of 10-MeC≡N-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> results in iminol 10-MeC(OH)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>, which, on treatment with a base, gives amide [10-MeC(=O)HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>]<sup>−</sup>. The reactions of 10-MeC≡N-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> with alcohols lead to imidates 10-ROC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> (R = Me, Et) as mixtures of <i>E</i>- and <i>Z</i>-isomers. In the solid state, 10-MeOC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> adopts <i>E</i>-configuration. The reactions of 10-MeC≡N-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> with primary amines result in amidines 10-RNHC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> (R = Me, Et) as mixtures of <i>E</i>- and <i>Z</i>-isomers. In the solid state 10-EtNHC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> was found to have the <i>Z</i>-configuration, which is stabilized by intramolecular N-H⋯H-B interactions between the NH group originating from the primary amine and the BH group of the carborane cage. These interactions are rather strong (3.7 kcal/mol) and are likely to persist in solution. The reactions of 10-MeC≡N-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> with secondary acyclic (Me<sub>2</sub>NH, Et<sub>2</sub>NH) and cyclic (piperidine, morpholine) amines result in amidines 10-R<sub>2</sub>NC(Me)=HN-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub> (R = Me, Et; R<sub>2</sub> = N(CH<sub>2</sub>)<sub>5</sub>, N(CH<sub>2</sub>CH<sub>2</sub>)<sub>2</sub>O) as single isomers, which, according to single crystal X-ray diffraction data, have the <i>E</i>-configuration.https://www.mdpi.com/1420-3049/30/4/828<i>nido</i>-carboraneacetonitrilium derivativeamideiminolimidatesamidines
spellingShingle Kirill R. Pakholkov
Ekaterina V. Bogdanova
Marina Yu. Stogniy
Kyrill Yu. Suponitsky
Sergey A. Anufriev
Igor B. Sivaev
Vladimir I. Bregadze
Nucleophilic Addition Reactions to 10-Acetonitrilium Derivative of <i>nido</i>-Carborane and Intramolecular NH⋯HB Interactions in <i>N</i>-Alkyl Amidines 10-RNHC(Me)=NH-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>
Molecules
<i>nido</i>-carborane
acetonitrilium derivative
amide
iminol
imidates
amidines
title Nucleophilic Addition Reactions to 10-Acetonitrilium Derivative of <i>nido</i>-Carborane and Intramolecular NH⋯HB Interactions in <i>N</i>-Alkyl Amidines 10-RNHC(Me)=NH-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>
title_full Nucleophilic Addition Reactions to 10-Acetonitrilium Derivative of <i>nido</i>-Carborane and Intramolecular NH⋯HB Interactions in <i>N</i>-Alkyl Amidines 10-RNHC(Me)=NH-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>
title_fullStr Nucleophilic Addition Reactions to 10-Acetonitrilium Derivative of <i>nido</i>-Carborane and Intramolecular NH⋯HB Interactions in <i>N</i>-Alkyl Amidines 10-RNHC(Me)=NH-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>
title_full_unstemmed Nucleophilic Addition Reactions to 10-Acetonitrilium Derivative of <i>nido</i>-Carborane and Intramolecular NH⋯HB Interactions in <i>N</i>-Alkyl Amidines 10-RNHC(Me)=NH-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>
title_short Nucleophilic Addition Reactions to 10-Acetonitrilium Derivative of <i>nido</i>-Carborane and Intramolecular NH⋯HB Interactions in <i>N</i>-Alkyl Amidines 10-RNHC(Me)=NH-7,8-C<sub>2</sub>B<sub>9</sub>H<sub>11</sub>
title_sort nucleophilic addition reactions to 10 acetonitrilium derivative of i nido i carborane and intramolecular nh⋯hb interactions in i n i alkyl amidines 10 rnhc me nh 7 8 c sub 2 sub b sub 9 sub h sub 11 sub
topic <i>nido</i>-carborane
acetonitrilium derivative
amide
iminol
imidates
amidines
url https://www.mdpi.com/1420-3049/30/4/828
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