A Catalytic Synthesis of Thiosilanes and Silthianes: Palladium Nanoparticle-Mediated Cross-Coupling of Silanes with Thio Phenyl and Thio Vinyl Ethers through Selective Carbon−Sulfur Bond Activation
作者:Mee-Kyung Chung、Marcel Schlaf
DOI:10.1021/ja049386u
日期:2004.6.1
Palladium nanoparticles generated in situ from N,N-dimethyl-acetamide (DMA) solutions of PdX2 (X = Cl-, OAc-, OCOCF3-) or Pd-2(dba)(3) by reduction with alkyl silanes R3SiH (R = Me, Et, i-Pr, t-Bu) are selective catalysts for the cross-coupling of the silanes R3SiH with phenyl and vinyl thioethers forming the corresponding thiosilanes and silthianes in high yields and under mild conditions. The method is applicable to phenyl thioglycosides, giving access to thiosilyl glycosides a new class of sugar derivatives.
METHODS FOR PREPARATION OF DISILATHIANES
作者:Thomas J. Curphey
DOI:10.1080/10426500108045265
日期:2001.8
Other methods investigated for the preparation of hexamethyldisilathiane included (a) reaction between commercial anhydrous Na2S and TMS chloride in N,N′-dimethylpropyleneurea or HMPA, (b) production of a highly-reactive Na2S by reaction between sodium dispersion and sulfur, followed by reaction with TMS chloride in THF at room temperature, and (c) reaction between sulfur, NaH, and TMS chloride in N