The reaction of di(tert-butyl)aluminium chloride with tert-butylhydrazine yielded an adduct (1) which was isolated in a pure form and characterized by crystal structure determination. 1 reacted with n-butyllithium by deprotonation and salt elimination to give the corresponding di(tert-butyl)aluminium hydrazide (2), which is a dimer in solution and in the solid state and possesses a four-membered Al2N2 heterocycle with two exocyclic N-N bonds. The structure of 2 differs from that of other di(tert-butyl)aluminium hydrazides which have four- or five-membered heterocycles. Treatment of impure samples of 1 with n-butyllithium yielded by the cleavage of the N-N bonds a mixture of several un-known products, from which the dimeric, centrosymmetric aluminium amide [(Me3C)(2)AlN(H)CMe3](2) (3) was isolated. A similar product (4) was obtained in a low yield by the reaction of (Me3SiCH2)(2)AlCl with the dilithium hydrazide Li2N2(SiMe3)(2). An intact N-N bond was neither found in the second product isolated from this reaction. Instead a tricyclic compound was formed by C-H activation which has two five-membered AlNSiC2 heterocycles bridged by Al-N bonds.
The reaction of di(tert-butyl)aluminium chloride with tert-butylhydrazine yielded an adduct (1) which was isolated in a pure form and characterized by crystal structure determination. 1 reacted with n-butyllithium by deprotonation and salt elimination to give the corresponding di(tert-butyl)aluminium hydrazide (2), which is a dimer in solution and in the solid state and possesses a four-membered Al2N2 heterocycle with two exocyclic N-N bonds. The structure of 2 differs from that of other di(tert-butyl)aluminium hydrazides which have four- or five-membered heterocycles. Treatment of impure samples of 1 with n-butyllithium yielded by the cleavage of the N-N bonds a mixture of several un-known products, from which the dimeric, centrosymmetric aluminium amide [(Me3C)(2)AlN(H)CMe3](2) (3) was isolated. A similar product (4) was obtained in a low yield by the reaction of (Me3SiCH2)(2)AlCl with the dilithium hydrazide Li2N2(SiMe3)(2). An intact N-N bond was neither found in the second product isolated from this reaction. Instead a tricyclic compound was formed by C-H activation which has two five-membered AlNSiC2 heterocycles bridged by Al-N bonds.