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首页> 外文期刊>Chemistry: A European journal >Synthesis, structure, and reactivity of a pyridine-stabilized germanone
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Synthesis, structure, and reactivity of a pyridine-stabilized germanone

机译：吡啶稳定的锗烷的合成，结构和反应活性

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摘要

The first isolable pyridine-stabilized germanone has been prepared and its reactivity toward trimethylaluminum has been investigated. The germanone adduct results from a stepwise conversion that starts from 4-dimethylaminopyridine (DMAP) and the ylide-like N-heterocyclic germylene LGe: (L=CH{(C=CH _2)(CMe)[N(aryl)]_2}, aryl=2,6-iPr_2C _6H_3) (1) at room temperature, and gives the corresponding germylene-pyridine adduct L(DMAP)Ge: (2) in 91 % yield. The latter reacts with N_2O at room temperature to form the desired germanone complex L(DMAP)Ge=O (3) in 73 % yield. The Ge-O distance of 1.646(2)?in 3 is the shortest hitherto reported for a Ge=O species. The reaction of 3 with trimethylaluminum leads solely to the addition product LGe(Me)O[Al(DMAP)Me _2] (4). The latter results from insertion of the Ge=O subunit into an Al-Me bond of AlMe_3 and concomitant migration of the DMAP ligand from germanium to the aluminum atom. Compounds 2-4 have been fully characterized by analytical and spectroscopic methods. Their molecular structures have been established by single-crystal X-ray crystallographic analysis. Heavy ketones: The 4-dimethylaminopyridine (DMAP)-supported germanone 2 has been prepared in a facile oxygenation of the DMAP germylene adduct 1 by N_2O. Compound 2 reacts as a germanone equivalent with trimethylaluminum to form the Ge=O addition product 3, in which the DMAP molecule has migrated from the germanium to the aluminum atom (see scheme; Ar=2,6-iPr_2C_6H _3, D=DMAP).
机译：制备了第一个可分离的吡啶稳定的锗烷，并研究了其对三甲基铝的反应性。锗烷加合物是由逐步转化产生的，该逐步转化起始于4-二甲基氨基吡啶（DMAP）和类似内酯的N-杂环亚甲基LGe：（L = CH {（C = CH _2）（CMe）[N（芳基）] _ 2} ，在室温下，芳基＝ 2，6-iPr_2C_6H_3）（1），以91％的收率得到相应的亚germ-吡啶加合物L（DMAP）Ge：（2）。后者在室温下与N_2O反应，以73％的收率形成所需的锗烷络合物L（DMAP）Ge = O（3）。 Ge-O距离1.646（2）？in 3是迄今为止报道的Ge = O物种中最短的距离。 3与三甲基铝的反应仅产生加成产物LGe（Me）O [Al（DMAP）Me _2]（4）。后者是由于Ge = O亚基插入AlMe_3的Al-Me键中以及DMAP配体从锗迁移到铝原子所致。化合物2-4已经通过分析和光谱法充分表征。它们的分子结构已经通过单晶X射线晶体学分析确定。重酮：在N_2O对DMAP次戊二烯加合物1进行简便的氧合反应中，制备了4-二甲基氨基吡啶（DMAP）负载的锗酮2。化合物2以锗烷当量的形式与三甲基铝反应形成Ge = O加成产物3，其中DMAP分子已从锗迁移到铝原子（参见示意图; Ar = 2,6-iPr_2C_6H _3，D = DMAP） 。

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