747-80-8Relevant academic research and scientific papers
Synthesis of Boron-Halogenated Diborylamines and Diborylhydrazines by Cleavage of Stannazanes
Diemer, Stefan,Noeth, Heinrich,Storch, Wolfgang
, p. 1765 - 1780 (2007/10/03)
The diborylamines R'-N(BRX)2 (3; X=Cl, Br) are obtained by stannazane cleavage of distannylorganylamines R'-N(SnMe3)2 (4) with alkyldihaloboranes RBX2 in a 1:2 molar ratio. The presence of the sterically demanding substituents R and R' also causes carbon-tin bond cleavage, resulting in low yields of 3. However, carbon-tin bond cleavage can be suppressed by the use of bis(dimethylchlorostannyl)organylamines 5 as the nitrogen source for the synthesis of diborylamines. This results in almost quantitative yields of the compounds 3. Treatment of the distannylhydrazines R2N-N(SnMe3)2 (7) with RBX2 in a 1:2 molar ratio leads to the formation of N,N-bis(alkylhaloboryl)hydrazines 8 under mild conditions and in good yield. The molecular structures of 3 and 8 were determined by multinuclear magnetic resonance spectra in solution as well as by X-ray structure analysis in the case of 8d. A typical structural feature of 8d is the intramolecular BN adduct formation. Support for the constitutions of compounds 8c comes from MS fragmentation patterns as well as from IR spectra.
1H and 13C NMR studies of η6-benzo-bonded (boron-nitrogen heteroarene)tricarbonylchromium complexes and related η6-phenyl-bonded (B, B', B''-trimethyl-N, N', N''-triarylborazine)-tricarbonylchromium complexes: crystallographic structure of a boron-nitrogen heteroarene
Allaoud, Smaiel,Conte, Seny,Fenet, Bernard,Frange, Bernard,Robert, Francis,et al.
, p. 59 - 68 (2007/10/02)
2,4-dimethyl-3-phenyl--7-chloro-8-methyl-2,4-dibora-1,3-diazaronaphthalene (C16H18B2N2Cl2) crystallizes in the monoclinic system: P2/a; a=8.149(3) Angstroem, b=13.379(3) Angstroem and c=15.193(3) Angstroem; β=91.03(2)o; Z=4; R=0.043; Rw=0.041.Reaction with gives exclusively the compounds with Cr(CO)3 η6-bonded to the benzo part of the molecule.This derivative is a 1:1 mixture of atropisomers which were partially separated and whose configurations could be deduced by means of solvent effects in nuclear magnetic resonance (NMR) spectroscopy.Similar results were obtained with 2,4-dimethyl-3-phenyl--6-chloro-8-methyl-2,4-dibora-1,3-diazaronaphthalene and although the separation of isomers failed.Additionally, two closely related η6-bonded isomers originating from the above ligands were identified in which the chlorine atom was replaced by a hydrogen atom.All these compounds were thoroughly characterized by high resolution 1H and 13C one-dimensional and 1H-1H nuclear Overhauser spectroscopy (NOESY) and correlated two-dimensional NMR spectroscopy (COSY).Further, the reaction of with B,B',B''-trimethyl-N,N',N''-triarylborazine, the phenyl bearing a para substituent (H, F or Me), was shown by 1H and 13C NMR spectroscopy to yield a compound with one phenyl group η6 bonded to Cr(CO)3.Key words: Chromium; Boron; Nuclear magnetic resonance
