Darstellung von m- und p-Phenylen-bis(dichlorstiban)/ Synthesis of m- and p-Phenylene-bis(dichlorostibane)

Abstract

Abstract The reaction of antimony(III)-chloride with lithiumdiisopropylamide in the molar ratio 1:2 in ether gives monochloro-bis(diisopropylamino)stibane (4). m -Bromophenyl-bis(diisopropylamino)stibane (2a) is prepared by reaction of m-bromophenyllithium with 4. p-Bromophenylbis(diisopropylamino)stibane (2b) can be obtained by reaction of p-brom ophenyl-dichlorostibane with lithium-diisopropylamide, or from p-brom ophenyllithium and 4. The metal-halogen-exchange of 2a, b by butyllithium in ether gives m- or p-Lithium phenyl-bis(diisopropylamino)- stibane (3a, b), respectively. Without isolation of the lithiated com pound m-/p-phenylene-bis[bis- (diisopropylamino)stibane] (5a, b) are prepared by reaction o f 3a, b with 4. Esterification of 5a, b with C2H5OH (1:4) yields m-/p-phenylene-bis(diethoxystibane) (6a, b). The reaction of 6a, b with acetylchloride in chloroform gives m -/p-phenylene-bis(dichlorostibane) (7a, b). The new compounds 2-7 are characterized by elemental analysis, NM R- and IR-spectra. 7a, b are also characterized by MS.