- Solubilizing functionalized molecular aluminosilicates
-
Molecular aluminosilicate LAl(SH)(μ-O)Si(OH)(OtBu) 21 (L = [HC{C(Me)N(Ar)}2]-, Ar = 2,6- iPr2C6H3) has been prepared from LAl(SH)22 and (tBuO)2Si(OH)2 in high yield. When reacted with one equiv. of water, the unique aluminosilicate containing two terminal hydroxy groups LAl(OH·THF)(μ-O)Si(OH)(O tBu)23 can be isolated. However, when 2 is reacted with the bulkier silanol (tBuO)3SiOH, no reaction is observed. The desired LAl(SH)(μ-O)Si(OtBu)36 can be prepared in a two-step synthesis between LAlH24 and (tBuO) 3SiOH giving first LAl(H)(μ-O)Si(OtBu)35, which reacts further with elemental sulfur to give 6 as the only product. Direct hydrolysis of 6 was conducted to obtain LAl(OH)(μ-O)Si(OtBu) 37, however, such hydrolysis always resulted in a complete decomposition of the starting material. Therefore we used boric acid, which condenses in non-polar solvents and slowly evolve water, to hydrolyze 6 to 7 under mild conditions. Compounds 1, 3 and 5-7 have been characterized by single-crystal X-ray diffraction. The Royal Society of Chemistry 2009.
- Rascon-Cruz, Fernando,Huerta-Lavorie, Raul,Jancik, Vojtech,Toscano, Ruben Alfredo,Cea-Olivares, Raymundo
-
p. 1195 - 1200
(2009/06/17)
-