(Ar); stirring at -78°C, heating at reflux temp. for 15 min.; product dissolved in sulfuric acid and precipitated with ice-water mixture;
参考文献
Diaz-Garcia, Maria A.; Agullo-Lopez, Fernando; Sastre, Angela; Torres, Tomas; Torruellas, William E.; Stegeman, George I.
Journal of Physical Chemistry, 1995 , vol. 99, # 41 p. 14988 - 14991
in diethyl ether byproducts: LiCl, AlCl3; distn. of BCl3 to water free etheric soln. of LiAlH4, cooled with liq. N2; heating up to room temp.; fractionated condensation;
参考文献
Journal of the American Chemical Society, , vol. 69, p. 1199 - 1203
(nC4H9)3SnH in neat (no solvent) condensing B compd. on top of tributyltin hydride at -196°C (molar ratio tin reagent/starting borane = 2.92); heating; stirring at 23°C, 12h; low temp. distn.; detn. by 1H, 2H, 11B NMR, IR spectroscopy;
Al or Ca or Mg or Na study of react. between 10 and 425°C; react. time 1-40 h; H2 pressure 140-250 bar; HBCl2 formed at iow temp., formation of B2H6, its pyrolysis products, and B2H5Cl above 100°C;
参考文献
Bulletin de la Societe Chimique de France, , p. 1367 - 1370
KH in dimethyl-ether byproducts: KHBCl3, H2; Me2O and B4H10 condensing onto KH at -196°C under N2, warming slowly to -45°C to remove all the volatiles, BCl3 condensing on theresidue at -196°C, stirring for 2.5-3 h at - 35°C coolingto -196°C, fractionating; identified by IR and NMR spectra;
in dichloromethane BCl3 condensing under N2 at -196°C onto phosphonium salt in CH2Cl2, warming to room temp., stirring for 2 h, cooling to -78°C, volatiles fractionating, diborane collecting at -196°C; identified by IR spectrum;
