Synthesis and structures of lithium N-trimethylsilyl- and -neopentyl-anilides and their Et_2O and tmen adducts; crystal structures of [(Li{#mu#-N(Ph)R}-trans)_2(#mu#-tmen)]_infinity (R = SiMe_3 1 or CH_2Bu~t 2) and [Li{#mu#-N(PH)CH_2Bu~t}(OEt_2)]_2

摘要

Treatment of N-trimethylsilyl- or -neopentyl-aniline successively with n-butyllithium and tmen in hexane yielded the crystalline polymeric lithium amides [(Li{#mu#-N(Ph)R}-trans)_2(#mu#-tmen)]_infinity (R = SiMe_3 1 or CH_2Bu~t 2), which contain the rare bridging, rather thanchelating, tmen ligands. Details are also provided of: (i) the preparation of crystalline [Li{N(Ph)SiMe_3}]_4, hydrocarbon-insoluble [Li{N(Ph)CH_2Bu~t}]_n, and diethyl ether aducts [Li{#mu#-N(Ph)R-trans}-(OEt_2)]_2 (R = SiMe_3 or CH_2Bu~t): (ii) variable temperature multinuclear NMR spectra in toluene-d_8 and (iii) three crystal structures.