FLP behaviour of cationic titanium complexes with tridentate Cp,O,N-ligands: highly efficient syntheses and activation reactions of C-X bonds (X = Cl, F)

Fischer Malte; Schwitalla Kevin; Baues Svenja; Schmidtmann Marc; Beckhaus Ruediger

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FLP behaviour of cationic titanium complexes with tridentate Cp,O,N-ligands: highly efficient syntheses and activation reactions of C-X bonds (X = Cl, F)

机译：阳离子钛配合物与三齿CP，O，N-配体的FLP行为：C-X键的高效合成和活化反应（x = Cl，F）

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The synthesis of cationic titanium complexes 4a,b with tridentate Cp,O,N-ligand frameworks, starting from the monopentafulvene complex Cp*Ti(Cl)(-(5):sigma-(1)-C5H4CR2 (CR2 = adamantylidene) (1) and bidentate O,N-ligand precursors CH3C(O)CH2CH2NR2 (R = Et, CH2Ph) (L1a,b), in a high-yielding and efficient two-step synthetic pathway is described. The -aminoketones L1a,b were synthesized by a herein reported solvent- and catalyst-free reaction. The reaction pathway involves insertion reactions, subsequent methylations and final activations with B(C6F5)(3). NMR investigations of the cationic titanium complex 4a in deuterated dichloromethane revealed an ongoing selective reaction under formation of the cationic complex 5a-d(2), which is the result of C-Cl bond cleavage. In addition to selective C-Cl bond activation reactions, C(sp(3))-F bonds were activated by 4a,b, pointing out the special tm-FLP nature of 4a,b.

机译：阳离子钛配合物4a，b的合成与三齿Cp，o，n-配体框架，从单opentafulvene络合物cp * ti（cl）开始（ - （5）：sigma-（1）-c5h4cr2（cr2 =亚氨基）（ 1）和二齿O，N-配体前体CH3C（O）CH 2 CH 2 CH 2 CH 2 CH 2 CH 2（R = ET，CH2PH）（L1A，B）在高产和有效的两步合成途径中进行了描述。-AMINOKETONE L1A，B是通过本文合成了报道的溶剂和催化剂反应。反应途径涉及插入反应，随后的甲基化和与B（C6F5）（3）的最终活性。阳离子钛络合物4a在氘代二氯甲烷中的NMR调查显示出持续的选择性反应在形成阳离子复合物5a-d（2）的下，这是C-C1键切割的结果。除了选择性C-Cl键活化反应外，C（SP（3）） - F键将4A， b，指出4a，b的特殊TM-FLP性质。

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《Dalton transactions: An international journal of inorganic chemistry》 |2019年第4期|共8页
作者
Fischer Malte; Schwitalla Kevin; Baues Svenja; Schmidtmann Marc; Beckhaus Ruediger;
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Carl von Ossietzky Univ Oldenburg Fak Math &

Nat Wissensch Inst Chem Postfach 2503 D-26111 Oldenburg Germany;

Carl von Ossietzky Univ Oldenburg Fak Math &

Nat Wissensch Inst Chem Postfach 2503 D-26111 Oldenburg Germany;

Carl von Ossietzky Univ Oldenburg Fak Math &

Nat Wissensch Inst Chem Postfach 2503 D-26111 Oldenburg Germany;

Carl von Ossietzky Univ Oldenburg Fak Math &

Nat Wissensch Inst Chem Postfach 2503 D-26111 Oldenburg Germany;

Carl von Ossietzky Univ Oldenburg Fak Math &

Nat Wissensch Inst Chem Postfach 2503 D-26111 Oldenburg Germany;

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中图分类化学;无机化学;
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1. FLP behaviour of cationic titanium complexes with tridentate Cp,O,N-ligands: highly efficient syntheses and activation reactions of C-X bonds (X = Cl, F) [J] . Fischer Malte, Schwitalla Kevin, Baues Svenja, Dalton transactions: An international journal of inorganic chemistry . 2019,第4期

机译：阳离子钛配合物与三齿CP，O，N-配体的FLP行为：C-X键的高效合成和活化反应（x = Cl，F）
2. Reaction of pentafulvene complexes of titanium with nitriles and iso-nitriles - Synthesis and isomerizations of sigma, pi-chelate complexes with Cp similar to N-ligands [German] [J] . Stroot J., Saak W., Haase D., Zeitschrift fur Anorganische und Allgemeine Chemie . 2002,第4期

机译：钛的五氟甲醚络合物与腈和异腈的反应-类似于N-配体的Cp的sigma，π-螯合物的合成和异构化[德国]
3. Strong Lewis acid air-stable cationic titanocene perfluoroalkyl(aryl)sulfonate complexes as highly efficient and recyclable catalysts for C–C bond forming reactions? [J] . Ningbo Li, Jinying Wang, Xiaohong Zhang, Dalton transactions: An international journal of inorganic chemistry . 2014,第30期

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4. C-H Bond Activation by Iridium and Rhodium Complexes: Catalytic Hydrogen-Deuterium Exchange and C-C Bond-Forming Reactions [C] . Steven R. Klei, Klan L. Tan, Jeffrey T. Golden, American Chemical Society National Meeting . 2004

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5. I. Synthesis and photophysical characterization of tridentate C^N*N platinum (II) complexes II. Investigation of selectivity in C--H bond activation by platinum. [D] . Ravindranathan, Deepak. 2012

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7. Formation of C-X Bonds through Stable Low-Electron-Count Cationic Platinum(IV) Alkyl Complexes Stabilized by N-Heterocyclic Carbenes [O] . Rivada Wheelaghan, Orestes, Roselló Merino, Marta, Díez Viñuela, Josefina Soledad, 2014

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机译：研究氢 - 氢和碳 - 硫键裂解;路易斯酸改性硫化钼配合物;和吡咯配合物的合成和反应。总结报告

FLP behaviour of cationic titanium complexes with tridentate Cp,O,N-ligands: highly efficient syntheses and activation reactions of C-X bonds (X = Cl, F)

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