A pentacoordinated norbornenyl-acyl-rhodium(III) complex as a likely intermediate in the catalytic hydroacylation of norbornadiene

Almenara N.; Ibarlucea L.; Mendicute-Fierro C.; Seco J. M.; Rodriguez-Dieguez A.; Garralda M. A.; Huertos M. A.

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A pentacoordinated norbornenyl-acyl-rhodium(III) complex as a likely intermediate in the catalytic hydroacylation of norbornadiene

机译：五配位的降冰片烯基-酰基-铑（III）配合物，可能是降冰片二烯催化加氢酰化反应的中间体

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[RhCl(NCO)(nbyl)(PR3)] (nbyl = sigma-norbornenyl; NCO = quinoline-8-acyl; R = p-F-C6H4) (1) has been synthesized by the reaction of [Rh(nbd) Cl](2) (nbd = norbornadiene) with 2 equivalents of NCHO (quinoline-8-carbaldehyde) and 2 equivalents of PR3. Compound 1 has been fully characterized in solution and also in the solid state by X-ray diffraction. Compound 1 shows low stability in solution and undergoes slow ring closure isomerization to [RhCl(NCO)(ntyl)(PR3)] (ntyl = sigma-nortricyclyl) (2) after 12 hours. Reaction of 1 with an extra equivalent of aldehyde (NCHO) and PR3 led to the formation of [RhCl(H)(NCO)(PR3)(2)] (3) and an equivalent of ketone, which is a hydroacylation product. The catalytic activity of 3 in the hydroacylation of nbd with NCHO is reported as well as the catalytic activity of compound 1. Compounds 1 and 3 are proposed as intermediate species in the catalytic hydroacylation of norbornadiene with NCHO.

机译：[RhCl（NCO）（nbyl）（PR3）]（nbyl = sigma-降冰片烯基; NCO =喹啉-8-酰基; R = pF-C6H4）（1）是通过[Rh（nbd）Cl]反应合成的（2）（nbd =降冰片二烯），含2当量的NCHO（喹啉-8-甲醛）和2当量的PR3。化合物1已经在溶液中以及在固态下通过X射线衍射被充分表征。化合物1在溶液中显示出低稳定性，并在12小时后缓慢闭环异构化为[RhCl（NCO）（ntyl）（PR3）]（ntyl = sigma-nortricyclyl）（2）。 1与额外当量的醛（NCHO）和PR3的反应导致形成[RhCl（H）（NCO）（PR3）（2）]（3）和当量的酮，后者是加氢酰化产物。报道了3在Nbd与NCHO加氢酰化中的催化活性以及化合物1的催化活性。提出了化合物1和3作为降冰片二烯与NCHO催化加氢酰化的中间体。

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《Dalton transactions: An international journal of inorganic chemistry》 |2016年第46期|共8页
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Almenara N.; Ibarlucea L.; Mendicute-Fierro C.; Seco J. M.; Rodriguez-Dieguez A.; Garralda M. A.; Huertos M. A.;
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1. A pentacoordinated norbornenyl-acyl-rhodium(III) complex as a likely intermediate in the catalytic hydroacylation of norbornadiene [J] . Almenara N., Ibarlucea L., Mendicute-Fierro C., Dalton transactions: An international journal of inorganic chemistry . 2016,第46期

机译：五配位的降冰片烯基-酰基-铑（III）配合物，可能是降冰片二烯催化加氢酰化反应的中间体
2. An Experimental and Theoretical Investigation on Pentacoordinated Cobalt(III) Complexes with an Intermediate S=1 Spin State: How Halide Ligands Affect their Magnetic Anisotropy [J] . Brazzolotto Deborah, Gennari Marcello, Yu Shengying, Chemistry: A European journal . 2016,第3期

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3. Structural, magnetic, and electronic properties of a pentacoordinated intermediate-spin (S=3/2) iron(III) complex with a macrocyclic [N-4](2-) ligand [J] . Keutel H., Jager EG., Grodzicki M., Inorganic Chemistry: A Research Journal that Includes Bioinorganic, Catalytic, Organometallic, Solid-State, and Synthetic Chemistry and Reaction Dynamics . 1999,第10期

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机译：开发人造蛋白酶和核酸酶：催化水解未活化的酰胺，腈和磷酸盐。第一部分钴（III）配合物促进的磷酸酯的水解。第二部分钴（III）配合物催化的腈水合。第三部分钴（III）配合物促进的酰胺水解。
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7. Catalytic Oxidation with a Non-Heme Iron Complex That Generates a Low-Spin FeIIIOOH Intermediate [O] . Roelfes Gerard, Lubben Marcel, Hage Ronald, 2000

机译：非血红素铁配合物催化氧化生成低旋转FeIIIOOH中间体

A pentacoordinated norbornenyl-acyl-rhodium(III) complex as a likely intermediate in the catalytic hydroacylation of norbornadiene

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