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Iron(II) Complexes of Chiral Tridentate Nitrogen Donors and their Application in Catalytic Hydrosilylation Reactions
Zeitschrift für anorganische und allgemeine Chemie ( IF 1.1 ) Pub Date : 2020-07-07 , DOI: 10.1002/zaac.201900310 Cedric Groß 1 , Andreas Omlor 2 , Tobias Grimm 1 , Benjamin Oelkers 1 , Yu Sun 1 , Volker Schünemann 2 , Werner R. Thiel 1
Zeitschrift für anorganische und allgemeine Chemie ( IF 1.1 ) Pub Date : 2020-07-07 , DOI: 10.1002/zaac.201900310 Cedric Groß 1 , Andreas Omlor 2 , Tobias Grimm 1 , Benjamin Oelkers 1 , Yu Sun 1 , Volker Schünemann 2 , Werner R. Thiel 1
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Enantiomerically pure, C2‐symmetric 2,6‐bis(pyrazol‐3‐yl) pyridine ligands were obtained by treatment of diethyl‐2,6‐pyridinedicarbonate with (1R,4R)‐(+)‐camphor in the presence of NaH followed by ring closure with hydrazine. After twofold N‐alkylation at the pyrazole rings, the addition of iron(II) chloride led to the according pentacoordinate dichloridoiron(II) complexes. All intermediates of the ligand synthesis, the ligands bearing NCH3 and NCH2C6H5 groups and the derived iron(II) complexes were structurally characterized by means of X‐ray structure analysis. In‐situ reaction with iron(II) carboxylates resulted in the formation of iron(II) carboxylate complexes, which turned out to be highly active in the hydrosilylation of acetophenone. However, even at room temperature, the enantiomeric excess of the product 1‐phenylethanol is poor. 57Fe Mössbauer spectroscopy gave an insight into the species formed during catalysis.
中文翻译：
手性三齿氮供体的铁（II）配合物及其在催化氢化硅烷化反应中的应用
对映体纯净的C 2对称的2,6-双（吡唑-3-基）吡啶配体是通过在存在下用（1 R，4 R）-（+）樟脑酸处理2,6-吡啶二碳酸二乙酯而得到的NaH 2，然后用肼进行闭环。在吡唑环上进行两次N-烷基化后，添加氯化铁（II）生成相应的五配位二氯亚铁（II）配合物。配体合成的所有中间体，带有NCH 3和NCH 2 C 6 H 5的配体X射线结构分析对基团和衍生的铁（II）配合物进行结构表征。与羧酸铁（II）的原位反应导致羧酸铁（II）配合物的形成，事实证明这在苯乙酮的氢化硅烷化中具有很高的活性。但是，即使在室温下，产物1-苯乙醇的对映体过量也很低。57 FeMössbauer光谱学深入了解了催化过程中形成的物质。
更新日期：2020-07-07
中文翻译：
手性三齿氮供体的铁（II）配合物及其在催化氢化硅烷化反应中的应用
对映体纯净的C 2对称的2,6-双（吡唑-3-基）吡啶配体是通过在存在下用（1 R，4 R）-（+）樟脑酸处理2,6-吡啶二碳酸二乙酯而得到的NaH 2，然后用肼进行闭环。在吡唑环上进行两次N-烷基化后，添加氯化铁（II）生成相应的五配位二氯亚铁（II）配合物。配体合成的所有中间体，带有NCH 3和NCH 2 C 6 H 5的配体X射线结构分析对基团和衍生的铁（II）配合物进行结构表征。与羧酸铁（II）的原位反应导致羧酸铁（II）配合物的形成，事实证明这在苯乙酮的氢化硅烷化中具有很高的活性。但是，即使在室温下，产物1-苯乙醇的对映体过量也很低。57 FeMössbauer光谱学深入了解了催化过程中形成的物质。
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