Synthesis, characterization and crystal structures of alkyl-, alkynyl-, alkoxo- and halo-magnesium amides
Resource
Journal of Organometallic Chemistry (648),176–187
Journal
Journal of Organometallic Chemistry (648),176–187
Pages
-
Date Issued
2002
Date
2002
Author(s)
Yang, Kuo-Ching
Chang, Chung-Cheng
Huang, Jyh-Yuan
Lee, Chih-Chien
Lin, Gene-Hsiang
Wang, Yu
Michael, Y.C.
DOI
246246/2006111501233244
Abstract
In our experiments, 1:1 stoichiometric reaction between MgR2 & diphenylamine produced the monomeric heteroleptic alkylmagnesium amides [RMgNPh2(THF)2] [R=Et 1 & iPr 2]. Adding the stronger donor solvent HMPA (HMPAhexamethylphosphoramide) to compound 1 caused disproportionation resulting in a bisamidomagnesium compound [Mg(NPh2)2(HMPA)2] 3. The stoichiometric reaction between bis(diisopropylamido)-magnesium & different substituted acetylenes HC CR in THF solution produced two dimeric amidomagnesium acetylide compounds [(RC C)Mg(-NiPr2)(THF)]2 [R=Ph 4, R=SiMe3 5]. When the differently sized secondary amines, HNEt2 & HN(SiMe3)2, were reacted with Grignard reagent EtMgBr, they produced diethylamino-bridging & bromo-bridging Hauser base [BrMg(-NEt2)(HMPA)]2 6 & [(Me3Si)2NMg(-Br)(OEt2)]2 7, respectively. Unexpectedly, the reaction of MgEt2 & HN(SiMe3)2 in refluxing THF produced [(Me3Si)2NMg(-OEt)(THF)]2 8. Additionally, we synthesized the first trinuclear magnesium compound [(tBuC C)(THF)Mg(-C CtBu)(-NiPr2)Mg(-C CtBu)(- NiPr2)Mg(THF)(C CtBu)] 9, which exhibited both an electron-rich bridging ligand NiPr2 & electron-deficient bridging ligand C CtBu. All of these new compounds (1–9) were characterized by 1H-, 13C-, 31P-NMR, IR spectroscopy, mass spectrometry & X-ray crystallography.
Subjects
Heteroleptic magnesium amides
Hauser base
Alkynyl-bridged trinuclear magnesium compound
Type
journal article
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