in gas High Pressure; reagents added to tube in dry ice bath, sealed in amts. to develop about 30-50 atm of pressure at 300°C, heated at 310-350°C for 1.5-69 h; analyzed by GLC;
in neat (no solvent) byproducts: HBr; heating of ferrosilicon with 25percent Fe in a N2 stream with Br2 vapor in a porcelaine tube at 800-850°C;; removal of Br2 by shaking with Hg; isolation by fractional distillation and condensation in vacuum;;
in neat (no solvent) The halogen was co-condensed in a flask at -196°C with the mixt. of SiF4 and SiF2 emerging out of the reactor tube; further products;; warmed to room temp.; the volatile products were sepd. and detected by NMR and MS;;
参考文献
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), , p. 1123 - 1126
