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  • Fluoro- and Chloroferrocene From 2-to 3-Substituted Derivatives
    Organometallics, 2018
    Co-Authors: Mehdi Tazi, Madani Hedidi, William Erb, Yury S. Halauko, Oleg A. Ivashkevich, Vadim E. Matulis, Thierry Roisnel, Vincent Dorcet, Ghenia Bentabed-ababsa, Florence Mongin
    Abstract:

    The ferrocene halogen "dance" has been deemed hardly controllable. Here, we describe the first efficient examples of this reaction. Conversion of 1-fluoro-2-iodo (or 1-chloro-2-iodo) to 1-fluoro-3-iodo (or 1-chloro-3-iodo) Ferrocenes was ensured by suitably protecting the free 5 position.

  • Fluoro- and Chloroferrocene: From 2- to 3‑Substituted Derivatives
    2018
    Co-Authors: Mehdi Tazi, Madani Hedidi, William Erb, Yury S. Halauko, Oleg A. Ivashkevich, Vadim E. Matulis, Thierry Roisnel, Vincent Dorcet, Ghenia Bentabed-ababsa, Florence Mongin
    Abstract:

    The ferrocene halogen “dance” has been deemed hardly controllable. Here, we describe the first efficient examples of this reaction. Conversion of 1-fluoro-2-iodo (or 1-chloro-2-iodo) to 1-fluoro-3-iodo (or 1-chloro-3-iodo) Ferrocenes was ensured by suitably protecting the free 5-position

  • From 2-to 3-Substituted Ferrocene Carboxamides or How to Apply Halogen "Dance" to the Ferrocene Series
    Organometallics, 2017
    Co-Authors: Mehdi Tazi, William Erb, Yury S. Halauko, Oleg A. Ivashkevich, Vadim E. Matulis, Thierry Roisnel, Vincent Dorcet, Florence Mongin
    Abstract:

    Two methods were compared to convert ferrocene into N,N-diisopropylferrocenecarboxamide, N,N-diethylferrocenecarboxamide, N,N-dimethylferrocenecarboxamide, and (4-morphohnocarbonyl)ferrocene, namely, deprotometalation followed by trapping using dialkylcarbamoyl chlorides and amide formation from the intermediate carboxylic acid. The four ferrocene-carboxamides were functionalized at C-2; in the case of the less hindered and more sensitive amides, recourse to a mixed lithium-zinc 2,2,6,6-tetramethylpiperidino-based base allowed us to "achieve the reactions. Halogen migration using lithium amides was next optimized. Whereas it appeared impossible to isolate the less hindered 3-iodoferrocenecarboxamides, 3-iodo-N,N-diisopropylferrocenecarboxamide proved stable and was converted to new 1,3-disubstituted Ferrocenes by Suzuki coupling or amide reduction. DFT calculations were used to rationalize the results obtained.

  • From 2- to 3‑Substituted Ferrocene Carboxamides or How to Apply Halogen “Dance” to the Ferrocene Series
    2017
    Co-Authors: Mehdi Tazi, William Erb, Yury S. Halauko, Oleg A. Ivashkevich, Vadim E. Matulis, Thierry Roisnel, Vincent Dorcet, Florence Mongin
    Abstract:

    Two methods were compared to convert ferrocene into N,N-diisopropyl­ferrocenecarboxamide, N,N-diethyl­ferrocene­carboxamide, N,N-dimethyl­ferrocene­carboxamide, and (4-morpholinocarbonyl)­ferrocene, namely, deprotometalation followed by trapping using dialkylcarbamoyl chlorides and amide formation from the intermediate carboxylic acid. The four ferrocenecarboxamides were functionalized at C2; in the case of the less hindered and more sensitive amides, recourse to a mixed lithium–zinc 2,2,6,6-tetramethylpiperidino-based base allowed us to achieve the reactions. Halogen migration using lithium amides was next optimized. Whereas it appeared impossible to isolate the less hindered 3-iodo­ferrocene­carboxamides, 3-iodo-N,N-diisopropyl­ferrocene­carboxamide proved stable and was converted to new 1,3-disubstituted Ferrocenes by Suzuki coupling or amide reduction. DFT calculations were used to rationalize the results obtained

  • Synthesis of ferrocene amides and esters from aminoferrocene and 2-substituted ferrocenecarboxylic acid and properties thereof
    New Journal of Chemistry, 2016
    Co-Authors: Palabindela Srinivas, Viatcheslav Jouikov, William Erb, Vincent Dorcet, Sunchu Prabhakar, Floris Chevallier, Ekhlass Nassar, Palakodety Radha Krishna, Florence Mongin
    Abstract:

    Different ferrocenecarboxamides were synthesized from aminoferrocene and various acid coupling partners such as N-alpha-Boc-L-tryptophan and N-protected sugar amino acids ( N-Boc-3-amino-3-deoxy-1,2-O-isopropylidene-alpha-D-ribofuranoic acid, N-Boc-3-amino-3-deoxy-1,2-O-isopropylidene-alpha-D-xylofuranoic acid and their corresponding homo- and hetero-dimers). Similarly, reactions between 2-aminoethyl ferrocenecarboxylate and N-protected sugar amino acids afforded compounds with a carboxamide functional group remotely positioned from the ferrocene core. The X-ray diffraction structure of one of them showed the presence of an intermolecular hydrogen bond between the amide functional groups. Carbonylamino ( or carbonyloxy) and oxycarbonyl 1,2-disubstituted Ferrocenes were prepared either as racemic mixtures or in enantiomerically pure ( S-P) form. Their electrochemical evaluation revealed distinctive features. Interestingly, the enantiomerically pure ferrocene diester showed a large potential shift (+45 mV) in the presence of L-glutamic acid. Finally, some of the synthesized Ferrocenes were evaluated for their antibacterial, antifungal and antiproliferative ( MCF-7) activities.

Toshikazu Hirao - One of the best experts on this subject based on the ideXlab platform.

  • intramolecular conformational control in Ferrocenes bearing podand dipeptide chains
    Organometallics, 2001
    Co-Authors: Toshiyuki Moriuchi, Akihiro Nomoto, And Kazuhiro Yoshida, Toshikazu Hirao
    Abstract:

    Ferrocenes bearing podand dipeptide chains were demonstrated to induce intramolecular conformational regulation through hydrogen bondings. The single-crystal X-ray structure determination of the ferrocene bearing the podand dipeptide chains -Gly-l-Pro-OEt confirmed the formation of two intramolecular interchain hydrogen bondings between CO (Gly) and NH (another Gly) of each podand dipeptide chain (N(1)···O(102), 2.910 A; N(101)···O(2), 2.898 A; N(201)···O(302), 2.85 A; N(301)···O(202), 2.87 A) to give a 10-membered hydrogen-bonded ring. The ferrocene bearing the podand dipeptide chains -l-Pro-Gly-OEt is also considered to form two rigid intramolecular interchain hydrogen bondings between CO (bridging) and NH (another Gly) to give a 14-membered hydrogen-bonded ring. Such an ordered conformation was supported by the induced circular dichroism. On the other hand, the ferrocene bearing one dipeptide chain -Gly-l-Pro-OEt is packed in a helically ordered arrangement with one turn of 15.65 A pitch height through...

  • chirality organization of Ferrocenes bearing podand dipeptide chains synthesis and structural characterization
    Journal of the American Chemical Society, 2001
    Co-Authors: Toshiyuki Moriuchi, Akihiro Nomoto, Kazuhiro Yoshida, And Akiya Ogawa, Toshikazu Hirao
    Abstract:

    A variety of Ferrocenes bearing podand dipeptide chains have been synthesized to form an ordered structure in both solid and solution states and have been investigated by 1H NMR, FT-IR, CD, and X-ray crystallographic analyses. Conformational enantiomerization through chirality organization was achieved by the intramolecular hydrogen bondings between the podand dipeptide chains. The single-crystal X-ray structure determination of the ferrocene 2 bearing the podand dipeptide chains (-d-Ala-d-Pro-OEt) revealed two C2-symmetric intramolecular hydrogen bondings between CO (Ala) and NH (another Ala) of each podand dipeptide chain to induce the chirality-organized structure. The molecular structures of the ferrocene 1 composed of the podand l-dipeptide chains (-l-Ala-l-Pro-OEt) and 2 are in a good mirror image relationship, indicating that they are conformational enantiomers. An opposite helically ordered molecular arrangement was formed in the crystal packing of 2 as compared with 1. The ferrocene 2 exhibited i...