Preparation of complex of germanium bichloride with 1,4-dioxane

Kolesnikov, S. P.; Rogozhin, I. S.; Нефедов, О. М.

doi:10.1007/bf00921313

Cited by 11 publications

(15 citation statements)

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“…Solvents were dried by standard methods and distilled prior to use. The starting materials were synthesized according to literature procedures: Ge[N(TMS) 2 ] 2 ,31 [GeCl 2 · C 4 H 8 O 2 ],32 LiN(TMS) 2 · Et 2 O,33 MeN(CH 2 CH 2 NHC 6 F 5 ) 2 ,34 BnN(CH 2 CH 2 NHC 6 F 5 ) 2 ,24b BnN(CH 2 CH 2 NHTMS) 2 ,24b H 2 (dpma),35 TMSN(CH 2 CH 2 NHTMS) 2 ,36 FcC(O)CH=CHPh,37 HN(C 6 F 5 ) 2 ,38 LiN(C 6 F 5 ) 2 ,38 and N , N′ ‐bis(pentafluorophenyl)benzene‐1,2‐diamine ( 1i ) 39. MeI (Aldrich), GeCl 4 (Aldrich), Et 2 S 2 (Aldrich), and 2,3‐dimethylbuta‐1,3‐diene (Aldrich) were distilled prior to use.…”

Section: Methodsmentioning

confidence: 99%

Stabilized Germylenes Based on Diethylenetriamines and Related Diamines: Synthesis, Structures, and Chemical Properties

et al. 2012

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A series of novel, low‐valent germanium compounds 2a–2j based on four diethylenetriamines 1a–1d, (methyl)bis(pyrrol‐2‐ylmethyl)amine (1e), N,N′‐(sulfanediyldibenzene‐2,1‐diyl)bis(pentafluoroaniline) (1f), N,N′‐(oxydibenzene‐2,1‐diyl)bis(pentafluoroaniline) (1g), and (pentafluorophenyl)amines 1i and 1j have been obtained either by the reaction of Ge[N(SiMe3)2]2 with various diamines (1a–1e) or by the metathesis reaction of [GeCl2·dioxane] with lithium amides. The oxidative insertion (with halogenation reagents, MeI, disulfides), [1+4] cycloaddition, and oxidation reactions of the synthesized germylenes were investigated. The compositions and structures of the novel compounds were established by elemental analysis, 1H and 13C NMR spectroscopy, and X‐ray diffraction analysis (germylenes 2b, 2i, 2j, Ge4+ compounds 5b, 7a, 7b, 8, 10, 11). All the synthesized germylenes are monomeric.

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Section: Methodsmentioning

confidence: 99%

Stabilized Germylenes Based on Diethylenetriamines and Related Diamines: Synthesis, Structures, and Chemical Properties

et al. 2012

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“…For facile handling of GeCl 2 for further reactions it is necessary to transfer it to a stable form to prevent polymerization. In 1974 Nefedov and co‐workers presented the GeCl 2 ⋅dioxane complex, which is a source of monomeric GeCl 2 and can be synthesized by reaction of trichlorogermane with an excess of dioxane . This GeCl 2 ⋅dioxane complex is a common precursor for further substitution or reductive coupling reactions.…”

Section: Divalent Halides Of Germanium Tin and Leadmentioning

confidence: 99%

“…In 1974 Nefedov and co-workers presented the GeCl 2 ·dioxane complex, which is as ource of monomeric GeCl 2 and can be synthesized by reaction of trichlorogermane with an excesso fd ioxane. [31] This GeCl 2 ·dioxane complex is ac ommonp recursor forf urther substitution or reductive coupling reactions. Startingf rom IPr-GeCl 2 (IPr = [(HCNDipp) 2 C];D ipp = 2,6-iPr 2 C 6 H 3 ), Rivard and coworkers developed an ew synthetic bottom-up method for the synthesis of oligomeric subhalides (GeCl 2 ) x (x !…”

Section: Pbxmentioning

confidence: 99%

“…Nevertheless,asubstitution of the Et 3 Pl igands is possible as the reactiono f1 with an excesso fa nother phosphine like nBu 3 Pl eads to the appearance of free Et 3 Pa sd etected by 31 PNMR spectroscopy of the reaction mixture ( Figure 16). This substitution reactionm ight therebyp roceed by ad issociative mechanism, since not enough space is left fora ni ncoming ligand as to be seen in the space-filling model in Figure14.…”

Section: First Trapped Intermediate Of the Disproportionation Reactiomentioning

confidence: 99%

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Halides of the Heavier Group 14 Homologues Germanium, Tin, and Lead—A Journey through Unusual Compounds and Oxidation States

Kunz

Schnepf

2018

Chemistry A European J

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Classical halides of the heavier Group 14 homologues germanium, tin, and lead are common precursors for the synthesis of exciting compounds, such as polyhedral clusters. To get access to larger metalloid cluster compounds of Group 14, the disproportionation reaction of metastable monohalide solutions, accessible through a preparative co‐condensation reaction, proved to be quite successful. As the identity of the subvalent halides within the metastable solutions were yet unknown the reaction course from a monohalide precursor to a metalloid cluster was mostly unidentified. This might change now, as a first subhalide cluster [Ge14Br8(Et3P)4] could be characterized, being the first trapped intermediate of the disproportionation reaction of Group 14 subhalides. All these aspects are included within this Minireview, together with a short historical overview, dealing with the development of the preparative co‐condensation technique out of the matrix isolation technique, being the essential first step of the synthesis of metastable monohalide solutions of the heavier Group 14 elements Ge and Sn.

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“…As was anticipated, the target pentagermapyramidane 1 was readily prepared by the straightforward reaction of the dioxane complex of dichlorogermylene GeCl 2 ·diox [11] with the dipotassium salt of the tetragermacyclobutadiene dianion {[(tBu 2 MeSi) 4 [12] Pentagermapyramidane 1 showed only one set of resonance signals for all four tBu 2 MeSi substituents in the NMR spectra ( 1 H, 13 C, 29 Si), indicative of its highly symmetrical composition in solution.…”

mentioning

confidence: 99%