DETERMINATION OF THE ABSOLUTE CONFIGURATIONS OF THE EPIMERS OF THE P-CHIRAL PHOSPHINE PH(2)PCH(2)CH(2)P-STAR-PH(L-(-)-MENTHYL) BY USE OF TWO-DIMENSIONAL NMR SPECTROSCOPY IN COMBINATION WITH A PALLADIUM(II) REPORTER COMPLEX

Jiang QZ.; Venanzi LM.; Ruegger H.

首页> 外文期刊>Journal of Organometallic Chemistry >DETERMINATION OF THE ABSOLUTE CONFIGURATIONS OF THE EPIMERS OF THE P-CHIRAL PHOSPHINE PH(2)PCH(2)CH(2)P-STAR-PH(L-(-)-MENTHYL) BY USE OF TWO-DIMENSIONAL NMR SPECTROSCOPY IN COMBINATION WITH A PALLADIUM(II) REPORTER COMPLEX

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DETERMINATION OF THE ABSOLUTE CONFIGURATIONS OF THE EPIMERS OF THE P-CHIRAL PHOSPHINE PH(2)PCH(2)CH(2)P-STAR-PH(L-(-)-MENTHYL) BY USE OF TWO-DIMENSIONAL NMR SPECTROSCOPY IN COMBINATION WITH A PALLADIUM(II) REPORTER COMPLEX

机译：二维核磁共振谱结合测定对-手性膦PH（2）PCH（2）CH（2）P-STAR-PH（L-（-）-薄荷基）的绝对构型含钯（II）报告化合物

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The two epimers of the new P-chiral phosphine Ph(2)PCH(2)CH(2)P*Ph(L-(-)-menthyl) (1-Rp and 1-Sp) were synthesized by treating Ph(2)PH with the diastereomerically pure forms of Ph(L-(-)-menthyl)CH=CH2)P. The palladium(II) complexes [Pd((S)-o-C(6)H(4)CHMeNMe(2))(1-Rp)][PF6], 2-Rp, and [Pd((S)-o-C(6)H(4)CHMeNMe(2))(1-Sp)[PF6], 2-Sp, were obtained by treating the corresponding bisphosphines with [Pd2Cl2((S)-o-C(6)H(4)CHMeNMe(2))(2)]. Each of these complexes exists in the form of two regioisomers differing in the orientation of the chiral phosphine relative to the C-donor. Constraints from close interligand, intramolecular hydrogen-hydrogen contacts within three of these palladium complexes were detected by two-dimensional NOE spectroscopy, and were used to determine the absolute configurations at the chiral phosphorus centers in the Ph(2)PCH(2)CH(2)PPh(L-(-)-menthyl) isomers. The conformations of the two chelate rings in the more abundant of these isomers were also determined. [References: 38]

机译：通过处理Ph（2）合成了新的P-手性膦Ph（2）PCH（2）CH（2）P * Ph（L-（-）-薄荷基）（1-Rp和1-Sp）的两个差向异构体）PH和非对映体纯净形式的Ph（L-（-）-薄荷基）CH = CH2）P。钯（II）络合物[Pd（（S）-oC（6）H（4）CHMeNMe（2））（1-Rp）] [PF6]，2-Rp和[Pd（（S）-oC（ 6）H（4）CHMeNMe（2））（1-Sp）[PF6]，2-Sp通过用[Pd2Cl2（（S）-oC（6）H（4）CHMeNMe（2）））（2）]。这些复合物中的每一种均以两种区域异构体的形式存在，其相对于C-供体的手性膦的取向不同。二维NOE光谱法检测了三个钯中的紧密配体，分子内氢-氢接触的约束，并通过二维NOE光谱法确定了Ph（2）PCH（2）CH（ 2）PPh（L-（-）-薄荷基）异构体。还确定了这些异构体中更丰富的两个螯合环的构象。 [参考：38]

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《Journal of Organometallic Chemistry》 |1995年第2期|共8页
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Jiang QZ.; Venanzi LM.; Ruegger H.;
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正文语种 eng
中图分类有机化学;
关键词
Chiral phosphine; Absolute configuration; Two-dimensional nmr; Palladium; Solution structure; Asymmetric hydrogenation; Metal-complexes; Molecular mechanics; Crystal-structure; Solid-state; Ligands; Catalysis; H-1; Homonuclear; Assignment;

机译：手性膦;绝对构型;二维核磁共振;钯;溶液结构;不对称氢化;金属络合物;分子力学;晶体结构;固态;配体;催化;H-1;单核;赋值;

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1. DETERMINATION OF THE ABSOLUTE CONFIGURATIONS OF THE EPIMERS OF THE P-CHIRAL PHOSPHINE PH(2)PCH(2)CH(2)P-STAR-PH(L-(-)-MENTHYL) BY USE OF TWO-DIMENSIONAL NMR SPECTROSCOPY IN COMBINATION WITH A PALLADIUM(II) REPORTER COMPLEX [J] . Jiang QZ., Venanzi LM., Ruegger H. Journal of Organometallic Chemistry . 1995,第1a2期

机译：二维核磁共振谱结合测定对-手性膦PH（2）PCH（2）CH（2）P-STAR-PH（L-（-）-薄荷基）的绝对构型含钯（II）报告化合物
2. Synthesis and reactivity studies of palladium(II) complexes containing the N-phosphorylated iminophosphorane-phosphine ligands Ph2PCH2P{=NP(=O)(OR)(2)}Ph-2 (R = Et, Ph): application to the catalytic synthesis of 2,3-dimethylfuran [J] . Cadierno V, Diez J, Garcia-Alvarez J, Dalton transactions: An international journal of inorganic chemistry . 2006,第47期

机译：含N-磷酸化亚氨基膦-膦配体Ph2PCH2P {= NP（= O）（OR）（2）} Ph-2（R = Et，Ph）的钯（II）配合物的合成和反应性研究：在催化合成中的应用2,3-二甲基呋喃
3. MULTINUCLEAR NMR SPECTROSCOPIC AND X-RAY CRYSTALLOGRAPHIC STUDIES OF A SERIES OF MERCURY(II) COMPLEXES CONTAINING THE BIDENTATE PHOSPHINE LIGAND PH2PCH2SI(CH3)(2)CH2PPH2 (L-2) [J] . Alyea EC., Shakya RP., Meehan PR., Inorganic Chemistry: A Research Journal that Includes Bioinorganic, Catalytic, Organometallic, Solid-State, and Synthetic Chemistry and Reaction Dynamics . 1997,第21期

机译：含二齿膦配体PH2PCH2SI（CH3）（2）CH2PPH2（L-2）的一系列汞（II）配合物的多核NMR光谱学和X射线晶体学研究
4. Protonation studies and the determination of self-exchange electron transfer rate constants using NMR spectroscopy for selected complexes of copper(II/I). [D] . Juntunen, Kerri Lynn. 1992

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5. Facile Arene LigandExchange in p-Cymene Ruthenium(II) Complexesof Tertiary P-Chiral Ferrocenyl Phosphines [O] . John Popp, Schirin Hanf, Evamarie Hey-Hawkins 2019

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机译：从双（膦）铂（II）， - 钯（II）和-Nickel（II）配合物中还原消除H-H，H-CH3和CH3-CH3：使用sCF-Xα-sW方法的理论研究

DETERMINATION OF THE ABSOLUTE CONFIGURATIONS OF THE EPIMERS OF THE P-CHIRAL PHOSPHINE PH(2)PCH(2)CH(2)P-STAR-PH(L-(-)-MENTHYL) BY USE OF TWO-DIMENSIONAL NMR SPECTROSCOPY IN COMBINATION WITH A PALLADIUM(II) REPORTER COMPLEX

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