Metallorganische Verbindungen, LV¹⁾ Donatorfreie tert.‐Butyl‐ und sek.‐Propylaluminium‐Verbindungen

Abstract

Tri-tert.-butylaluminium (1) und Tri-2-propylaluminium (2) lassen sich aus Aluminiumchlorid oder den entsprechenden Dialkylaluminiumfluoriden 3 bzw. 6 und Alkyllithium in Ausbeuten zwischen etwa 60 und 90% isomerenfrei darstellen. Aus den Atheraten von 1 und 2, die aus atherischen Losungen von Grignardverbindungen und Aluminiumchlorid leicht zuganglich sind, werden die Dialkylaluminiumfluoride 3 und 6 durch Reaktion mit Borfluorid erhalten. Die Alkylaluminiumchloride 8 bis 11 mit tert.-Butyl-oder Isopropylresten sind aus 1 bzw. 2 und Aluminiumchlorid (Molverhaltnis 2:l oder 1 : 2) leicht zuganglich. Organometallic Compounds, LV l) -Donor-free tert-Butyl-and sec-Propylaluminium CompoundsTri-tert-butylaluminium (1) and tri-2-propylaluminium (2) can be prepared free from isomers and in 60-90 % yield by reaction of aluminium chloride or the corresponding dialkylaluminium fluorides 3 and 6, respectively, with alkyllithium. The dialkylaluminium fluorides 3 and 6 can be obtained by reaction of the etherate of boron fluoride with the etherates of 1 and 2, which are available from aluminium chloride and the corresponding alkylmagnesium chlorides. The alkylaluminium chlorides 8 to 11 containing tert-butyl and isopropyl groups are formed by reaction of 1 and 2, respectively, with aluminium chloride in molar ratios of 2:l or 1:2.In einer fruheren Arbeit3) uber die Synthese von tert.-Butyl-und Isopropylaluminium-atheraten wurde kurz erwahnt, dalj es uns gelungen sei, donatorfreies Tritert.-butylaluminium durch Reaktion von tert.-Butyllithium mit Aluminiumchlorid darzustellen.In Fortsetzung dieser Arbeit haben wir auf verschiedenen Wegen versucht, Tritat.-butylaluminium (1) und Tri-2-propylaluminium (2) moglichst frei von den Iso-

tBuP(NH2)2—A Reactive Synthon for the Synthesis of Molecular Imidophosphinates of Group 13 Metals

“…Solvents were distilled from sodium benzophenone ketyl or Na/K alloy prior to use. tBuP(NH 2 ) 2 , [6] GaMe 3 , [19] InMe 3 , [20] AltBu 3 [21] and Ga(tBu) 3 [22] were prepared according to literature methods, whereas AlMe 3 was commercially available (Aldrich) and used as received. NMR spectra were recorded using a Bruker DPX 300 spectrometer.…”

Structural characterization of a completely alkyl-substituted Al–Sb Lewis acid–base adduct

“…t-Bu 3 Al [14] and Me 3 Sb [15] were prepared according to literature methods. 1 H and 13 C{ 1 H} spectra were recorded using a Bruker AMX 300 spectrometer and are referenced to internal C 6 D 5 H (d 1 H 7.154, d 13 C 128.0).…”

The first 1,3,2-diazaalumina-[3]ferrocenophanes

“…Because of the availability of 1,1 0 -diaminoferrocene [6,7], and its N,N 0 -bis(trimethylsilyl) derivative 1 [7], the synthesis of 1,n-diaza-[n]ferrocenophanes with N-trimethylsilyl groups and various heteroatoms in the bridge has become an attractive goal [8][9][10][11][12][13]. In this work, we have studied the reaction of the dilithiated derivative 2 with RAlCl 2 3 in the presence of pyridine (py) [3a (R = t Bu) [14], 3b (R = CH(SiMe 3 ) 2 ) [15], 3c (R = C(SiMe 3 ) 3 ) [16], and 3d (R = Si(SiMe 3 ) 3 ) [15]] as the THF or pyridine adduct (Scheme 1).…”