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Extra resources for Organosilicon Chemistry. Special Lectures Presented at the International Symposium on Organosilicon Chemistry
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Organometal. Chem. 2, 129 (1964). 2 3 33 D SILATRANES: INTRA-COMPLEX HETEROCYCLIC COMPOUNDS OF PENTACOORDINATED SILICON M. G. VORONKOVf Institute of Organic Synthesis, Academy of Sciences of the Latvian SSR, Riga {USSR) In recent years a number of authors have evinced interest in intra-complex heterocyclic inorganic esters and alcoholates of triethanolamine and its derivatives of the type R w- 3 M ( O C H 2 C H 2 ) 3 N ( I ) , where M = an atom t ι of tri- or multivalent element with an incomplete p - or ^/-valency shell; η = its valency; and R = an organic radical, hydrogen or any other substituent.
O R G A N O M E T A L L I S C H E V E R B I N D U N G E N DES Si, Ge, UND Sn [(CH 3 )2GeCl] 3 N + 3 L i C H 3 > [ ( C H 3) 3G e ] 3N + ( C H 3 ) 3 G e O C 6 H 5 + NaNH 2 > ( C H 3) 3G e N H 2 + N a O C 6H 5 3 ( G H 3) 3G e N H 2 3LiCl > [ ( C H 3 ) 3 G e ] 3 N + 2NH 3 Diese unzersetzt destillierbare und schön kristallisierende Verbindung ist zwar nicht, wie die entsprechende Siliziumverbindung, gegen Wasser beständig, aber auch nicht so extrem hydrolyseempfindlich wie die anderen Methylgermanylamine.
The synthesis is achieved by preparing an equimolecular mixture of tetraethoxysilane (or tetramethoxysilane), triethanolamine, a corresponding alcohol or phenol and a catalyst; the whole mixture is then heated until ethanol (or methanol) is completely distilled off (0-5-1-5 h). 1-Organoxysilatranes are crystallized directly from the reaction mixture or are separated from it after evaporation of the solvent and then purified by recrystallization. 1-Alkoxy- and 1-cycloalkoxysilatranes are crystallized from tt-heptane (1-methoxy- and 1-cyclohexoxy derivatives can be also crystallized from xylene), and 1-aralkoxy- and 1-aroxysilatranes from xylene, a mixture of chloroform and rc-heptane, or from carbon tetrachloride and chloroform.