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Synthesis, structure and thermolysis of oxazagermines and oxazasilines

NJC17

F. Dannenberg, G. Thiele, E. Dornsiepen, S. Dehnen, M. Mehring – 2017

Seven new spirocyclic amido alkoxides of silicon and germanium were synthesized by the reactions of substituted 2-(aminomethyl)phenols with silicon(IV) and germanium(IV) chloride, respectively. The spirocyclic compounds 1–7 exhibit the general structural motif M[OC6H3(CH2NR1)-2-R2-4]2 [M = Si, R1 = Ph, R2 = H (1), Me (2), Br (3); M = Ge, R1 = Ph, R2 = H (4), Me (5), Br (6); M = Ge, R1 = i-Pr, R2 = H (7)]. The use of 2-(ethylamino)benzylalcohol and germanium(IV) chloride as starting materials afforded the spirocyclic compound Ge[EtNC6H4(CH2O)-2]2 (8). The structurally related germylene, germanium(II)-2-(phenylamidomethyl)phenolate (9), was prepared by the reaction of Ge[N(SiMe3)2]2 with 2-(phenylaminomethyl)phenol. The tetravalent compounds were isolated as racemates, with the exception of the spirocyclic germanium compound 8, for which the R and the S isomers crystallized separately. The compounds were characterized by single-crystal X-ray diffraction analysis, NMR spectroscopy (1H, 13C{1H}, 29Si{1H} for 1–3), IR spectroscopy, and TGA analysis. Porous Ge@C composites were observed after the carbonization of compounds 4–9 under argon. The as-prepared Ge@C materials were analyzed by elemental analysis, nitrogen physisorption measurements, powder X-ray diffraction analysis, Raman spectroscopy, and SEM/EDX analysis.

Title
Synthesis, structure and thermolysis of oxazagermines and oxazasilines
Author
F. Dannenberg, G. Thiele, E. Dornsiepen, S. Dehnen, M. Mehring
Date
2017
Citation
New J. Chem. 2017, 41, 4990.
Type
Text