ic000234j_si_001.pdf (768.69 kB)
Download fileSynthesis and Characterization of a Series of Zinc Bis[(alkyl)(trimethylsilyl)amide] Compounds
journal contribution
posted on 2000-11-10, 00:00 authored by David A. Gaul, Oliver Just, William S. ReesA series of 21 secondary (alkyl)(trimethylsilyl)amines HNR(TMS) [R = n-propyl (1), i-propyl (2), n-butyl (3),
i-butyl (4), s-butyl (5), tert-butyl (6), c-pentyl (7), n-pentyl (8), i-pentyl (9), 1-methylbutyl (10), 2-methylbutyl
(11), 1-ethylpropyl (12), 1,2-dimethylpropyl (13), tert-pentyl (14), phenyl (15), c-hexyl (16), n-hexyl (17), N,N-dimethyl-3-aminopropyl (18), benzyl (19), n-heptyl (20), 1,1,3,3-tert-butyl (21); TMS = Si(CH3)3] has been prepared
and fully characterized by elemental analyses, multinuclear (1H, 13C, 29Si, 14N) NMR, IR, UV/vis, MS, and boiling
point. A new method for determination of boiling points of milligram-size samples, based on DSC (differential
scanning calorimetry), is described. Each amine has been converted to the corresponding zinc bis(amide) compound
Zn[N(TMS)(R)]2 [R = n-propyl (22), i-propyl (23), n-butyl (24), i-butyl (25), s-butyl (26), tert-butyl (27), c-pentyl
(28), n-pentyl (29), i-pentyl (30), 1-methylbutyl (31), 2-methylbutyl (32), 1-ethylpropyl (33), 1,2-dimethylpropyl
(34), tert-pentyl (35), phenyl (36), c-hexyl (37), n-hexyl (38), N,N-dimethyl-3-aminopropyl (39), benzyl (40),
n-heptyl (41), 1,1,3,3-tert-butyl (42); TMS = Si(CH3)3] and subsequently fully characterized by elemental analyses,
multinuclear (1H, 13C, 29Si, 14N) NMR, IR, UV/vis, MS, and TGA. The experimental IR has been compared to
the computationally calculated one for compound 27. Observed trends in volatility of the compounds are discussed
in the context of the dominant intermolecular forces present in the condensed phase.