in dichloromethane WCl6 suspd. in CH2Cl2, soln. of Si compd. in CH2Cl2 added over a 4-h period under N2; filtration, washing with pentane, drying in vac., removal of CH2Cl2 from filtrate in vac., sublimation at 80°C;
参考文献
Pederson,S.F.; Schrock,R.R.
Journal of the American Chemical Society, 1982 , vol. 104, p. 7483
in neat (no solvent) byproducts: NOCl, CCl4; under exclusion of moisture, refluxed for 10 min, cooled quickly to 0°C; filtered; dried under vac.; elem. anal.;
参考文献
Prinz, H.; Dehnicke, K.; Mueller, U.
Zeitschrift fuer Anorganische und Allgemeine Chemie, 1982 , vol. 488, p. 49 - 59
carboxylic acids in benzene react. of WCl6 with carboxylic acids forming WOCl4 and acyl chlorides; not isolated, monitored by UV and IR;
参考文献
Lappert, Michael F.; Raston, Colin L.; Rowbottom, Graham L.; Skelton, Brian W.; White, Allan H.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1984 , p. 883 - 892
in neat (no solvent, solid phase) by react. of W-compd. with As2O3 at 100°C in a sealed tube;; resublimation at 120°C; elem. anal.;;
参考文献
Drew, Michael G. B.; Page, Elizabeth M.; Rice, David A.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1983 , p. 61 - 64
reaction of WCl6 with W at 270-750°C for 14 h under a vacuum; removal of WCl4 and WOCl4 byproducts by sublimation, intermediate (H3O)2W6Cl14*6H2O obtained after recrystn. from boiling HCl and cooling to -10°C; intermediate heated at 450°C under a dynamic vacuum;
参考文献
Rauch; DiSalvo; Zhou; Tang; Edwards
Journal of Alloys and Compounds, 1992 , vol. 182, # 2 p. 253 - 264
