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Nobuaki Kambe - One of the best experts on this subject based on the ideXlab platform.

Jun Terao - One of the best experts on this subject based on the ideXlab platform.

Viatcheslav Jouikov - One of the best experts on this subject based on the ideXlab platform.

  • Nucleophilic displacement versus electron transfer in the reactions of alkyl Chlorosilanes with electrogenerated aromatic anion radicals
    Electrochimica Acta, 2015
    Co-Authors: Saida Soualmi, Mamadou Dieng, Ali Ourari, Diariatou Gningue-sall, Viatcheslav Jouikov
    Abstract:

    Anion radicals of a series of aromatic compounds (C6H5CN, C6H5COOEt, anthracene, 9,10-dimethyl-, 9,10-diphenyl- and 9-phenylanthracene, pyrene and naphthalene) react with trialkyl Chlorosilanes R1R2R3SiCl (R1-3 = Me, Et; R1,2 = Me, R3 = t-Bu) in multiple ways, following classical bimolecular schemes. The ratio of one-electron transfer (ET) to a two-electron process (SN2-like nucleophilic attack of the reduced form of mediator on the chlorosilane, with k2 ≅ 102-108 M−1 s−1) is inversely related to the steric availability of Si for nucleophilic displacement reactions. The nucleophilic substitution pathway mainly results in mono- and disilylated aromatic products. Paralleling the electrochemical data with DFT calculations, the role of silicophilic solvent (DMF) in SN process was shown to be quite complex because of its involvement into coordination extension at silicon, dynamically modifying energetics of the process along the reaction coordinate. Although 2,2'-bipyridine also forms delocalized persistent anion radicals, they do not induce neither ET nor SN reactions in the same manner as aromatic mediators. Silicophilicity of 2,2'-bipyridine being superior to that of DMF, a R3SiCl·bipy complex of hypercoordinated silicon with electroactive ligand was formed instead, whose reduction requires about 1 V less negative potentials than bipyridine itself.

Richard A Register - One of the best experts on this subject based on the ideXlab platform.

  • strategies for the synthesis of well defined star polymers by anionic polymerization with chlorosilane coupling and preservation of the star architecture during catalytic hydrogenation
    Macromolecules, 2016
    Co-Authors: Adam B Burns, Richard A Register
    Abstract:

    The synthesis of isoprene-based star polymers by anionic polymerization, chlorosilane coupling, and catalytic hydrogenation was studied in detail, with the goal of obtaining and preserving a well-defined star architecture. The coupling reaction between polyisoprenyllithium (PI-Li) and Chlorosilanes, which can be intractably slow in apolar media, was dramatically accelerated by the concurrent addition of tetrahydrofuran (THF) with the coupling agent. In the presence of THF, PI-Li produces a yellow color allowing the living end concentration to be tracked visually, enabling near-stoichiometric coupling, as demonstrated by the synthesis of 6-arm star polymers and star block copolymers. Moreover, glassblowing techniques are not required. Star polymers coupled with chlorosilane terminating agents lost arms during catalytic hydrogenation. Several common hydrogenation catalysts were evaluated. The degree of degradation depended on the identity of the catalyst and the temperature of the reaction—more active catal...

  • Strategies for the Synthesis of Well-Defined Star Polymers by Anionic Polymerization with Chlorosilane Coupling and Preservation of the Star Architecture during Catalytic Hydrogenation
    2016
    Co-Authors: Adam B Burns, Richard A Register
    Abstract:

    The synthesis of isoprene-based star polymers by anionic polymerization, chlorosilane coupling, and catalytic hydrogenation was studied in detail, with the goal of obtaining and preserving a well-defined star architecture. The coupling reaction between poly­isoprenyl­lithium (PI-Li) and Chlorosilanes, which can be intractably slow in apolar media, was dramatically accelerated by the concurrent addition of tetrahydrofuran (THF) with the coupling agent. In the presence of THF, PI-Li produces a yellow color allowing the living end concentration to be tracked visually, enabling near-stoichiometric coupling, as demonstrated by the synthesis of 6-arm star polymers and star block copolymers. Moreover, glassblowing techniques are not required. Star polymers coupled with chlorosilane terminating agents lost arms during catalytic hydrogenation. Several common hydrogenation catalysts were evaluated. The degree of degradation depended on the identity of the catalyst and the temperature of the reactionmore active catalysts and higher temperatures led to more scissionbut not the reaction time. Degradation closely tracked the hydrogenation reaction indicating that scission is a catalytically activated process. This phenomenon is attributed to a decreasing affinity of the polymer for the catalyst with increasing saturation. Degradation of the star architecture depended strongly on the steric environment at the core. It was shown that the steric strain can be reduced by tuning the topology of the coupling agent to limit the number of arms per Si atom. The steric constraints at the core were further relaxed by adding a short run of butadiene units to the arms just prior to coupling, which nearly eliminated degradation during hydrogenation of a 6-arm star

Bogdan Marciniec - One of the best experts on this subject based on the ideXlab platform.

  • Iridium-Promoted Conversion of Chlorosilanes to Alkynyl Derivatives in a One-Pot Reaction Sequence
    Organometallics, 2014
    Co-Authors: Ireneusz Kownacki, Bartosz Orwat, Bogdan Marciniec
    Abstract:

    By making use of the catalytic potential of the iridium system [{Ir(μ-Cl)(CO)2}2]/NEt(i-Pr)2 in the synthesis of silyl-functionalized alkynes via silylative coupling of terminal alkynes/diynes with iodosilanes, we propose a new protocol allowing employment of various mono- and diChlorosilanes as reagents. The process is based on a sequence of two reactions occurring simultaneously: i.e., conversion of initial chlorosilane (SiR1nCl4–n) to the appropriate iodosilane via Cl/I nucleophilic substitution and its further conversion to a silylalkyne derivative ((SiR1n(C≡CR2)4–n) via iridium-catalyzed silylative coupling with terminal alkyne. Under optimum conditions, the method has proved to be effective and versatile in the conversion of a wide range of Chlorosilanes to a rich portfolio of various corresponding alkynyl-functionalized silicon derivatives. Additionally, NMR studies of the equimolar reaction of a well-defined iridium(I) alkynyl precursor with Me3Si–I revealed that ≡Si–I bond activation in iodosilan...

  • Iridium-Promoted Conversion of Chlorosilanes to Alkynyl Derivatives in a One-Pot Reaction Sequence
    2014
    Co-Authors: Ireneusz Kownacki, Bartosz Orwat, Bogdan Marciniec
    Abstract:

    By making use of the catalytic potential of the iridium system [{Ir­(μ-Cl)­(CO)2}2]/NEt­(i-Pr)2 in the synthesis of silyl-functionalized alkynes via silylative coupling of terminal alkynes/diynes with iodosilanes, we propose a new protocol allowing employment of various mono- and diChlorosilanes as reagents. The process is based on a sequence of two reactions occurring simultaneously: i.e., conversion of initial chlorosilane (SiR1nCl4–n) to the appropriate iodosilane via Cl/I nucleophilic substitution and its further conversion to a silylalkyne derivative ((SiR1n(CCR2)4–n) via iridium-catalyzed silylative coupling with terminal alkyne. Under optimum conditions, the method has proved to be effective and versatile in the conversion of a wide range of Chlorosilanes to a rich portfolio of various corresponding alkynyl-functionalized silicon derivatives. Additionally, NMR studies of the equimolar reaction of a well-defined iridium­(I) alkynyl precursor with Me3Si–I revealed that Si–I bond activation in iodosilane molecules occurred via oxidative addition to the iridium center