二氯(二异丙基氨基)硼烷合成路线 (共 15 条)
反应条件
in diethyl ether
(N2) or (Ar); addn. of Mg(C4H6)*2THF in portions to soln. of (iPr)2NBCl2 at -80°C within 1 h under stirring; stirring at -80°C for 2 h; slowly warming to 20°C; stirring overnight; filtration; washing with Et2O; evapn. of Et2O-soln. and then distn. in vac.; condensation; elem. anal.;
参考文献
Herberich, Gerhard E.; Boveleth, Wilfried; Hessner, Bernd; Hostalek, Martin; Koeffer, Dieter P. J.; et al.
Chemische Berichte, 1986 , vol. 119, # 2 p. 420 - 433
反应条件
Na#K in hexane
byproducts: NaCl, KCl; (under N2) to stirred Cl2BN(i-Pr)2 in hexane 1,3-butadiene is added (-40°C), after stirring for 3 h the cool mixt. is added at 20°C to Na/K-alloy in hexane (10 min, low temp.-condenser) on applying warm air the mixt. starts to reflux (3 h); filtn. under pressure, hexane is distd. off, distn., elem. anal.;
参考文献
Bromm, Dietmar; Stalke, Dietmar; Heine, Andreas; Meller, Anton; Sheldrick, George M.
Journal of Organometallic Chemistry, 1990 , vol. 386, # 1 p. 1 - 7
反应条件
n-butyllithium in hexane
n-BuLi in hexane added to soln. of TMEDA in hexane at room temp. under N2, stirred for 30 min, furan added, stirred for 90 min, Cl2BN(C3H7)2 in hexane added to the reaction mixture at -25°C, allowed to warm, and stirred for 20 h at room temp.; volatiles removed in vacuum, residue dissolved in hexane, filtered, solvent evapn. in vacuum, product distilled;
参考文献
Koehler, Thomas; Faderl, Juergen; Pritzkow, Hans; Siebert, Walter
European Journal of Inorganic Chemistry, 2002 , # 11 p. 2942 - 2946
反应条件
in hexane
byproducts: KCl; addn. of a soln. of (i-Pr)2NBCl2 to a suspn. of K2(t(-BuP)4) at -78.degrree.C, warming to 10°C within 12 h; filtn., washing with n-hexane, removal of the solvent, cooling to -20°C, filtn., elem. anal.;
参考文献
Riegel, B.; Pfitzner, A.; Heckmann, G.; Binder, H.; Fluck, E.
Zeitschrift fuer Anorganische und Allgemeine Chemie, 1994 , vol. 620, p. 8 - 15
反应条件
in pentane
under N2, borane layered with diimide, stirred for 15 h; removal of volatiles in vac., taken up in pentane, filtered, evapd., cooled to -30°C,; elem. anal.;
参考文献
Schmid, Guenter; Gehrke, Helmut; Kolorz, Hans-Ulrich; Boese, Roland
Chemische Berichte, 1993 , vol. 126, # 8 p. 1781 - 1786