in ethylene glycol dimethyl ether React. of starting materials in glyme.; Immersing of react. flask in oil bath and cooling (0°C). While react. is pumped under dynamic vac., the temp. of oil bath is slowly raised to 45°C, maintained there for 3 h, and then to 110°C (3h). B10H14 is obtained after cooling.;
参考文献
Lawrence, Steven H.; Wermer, Joseph R.; Boocock, Simon K.; Banks, Michael A.; Keller, Phillip C.; Shore, Sheldon G.
Inorganic Chemistry, 1986 , vol. 25, p. 367 - 372
in neat (no solvent) excess BCl3 condensed onto CrOF4 at -196°C and mixt. allowed to warm to room temp.;
参考文献
Hope, Eric G.; Jones, Peter J.; Levason, William; Ogden, J. Steven; Tajik, Mahmoud; Turff, Jeremy W.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1985 , p. 529 - 534
AlCl3; Me2NTol in dichloromethane 1:1 mixt. of BCl3 and AlCl, pinacol (2.3-3.0 equiv.) and lutidine (15 equiv.) for 18 h;
参考文献
Del Grosso, Alessandro; Helm, Matthew D.; Solomon, Sophia A.; Caras-Quintero, Dolores; Ingleson, Michael J.
Chemical Communications, 2011 , vol. 47, # 46 p. 12459 - 12461
in neat (no solvent, gas phase) Electric Arc; Ar; a gas mixt. at 40 psi pressure injected with a pulsed mol. beam valve (General Valve, series 9) into a flow channel prior to supersonic expansion into a vac. chamber, struck a discharge between a pair of stainless steel ring electrodes;
参考文献
He, Sheng-Gui; Clouthier, Dennis J.; Adam, Allan G.; Tokaryk, Dennis W.
Journal of Chemical Physics, 2005 , vol. 122, # 19 art. no. 194314
AlCl3; 2,6-lutidine in dichloromethane 1:1 mixt. of BCl3 and AlCl, pinacol (2.3-3.0 equiv.) and lutidine (15 equiv.) for 14 h;
参考文献
Del Grosso, Alessandro; Helm, Matthew D.; Solomon, Sophia A.; Caras-Quintero, Dolores; Ingleson, Michael J.
Chemical Communications, 2011 , vol. 47, # 46 p. 12459 - 12461
