hydrogenchloride in diethyl ether under N2; to cold (-78 °C) soln. of boron compd. in Et2O slowly added MeLi, stirred for 0.5 h, warmed to room temp., stirred for 0.5 h,Li(BMe4) detected by (11)B NMR, cooled to 0 °C, added soln. of HCl in Et2O, stirred for 15 min, warmed; not isolated, monitored by (11)B NMR;
in neat (no solvent) Sonication; (N2), Et3Al introduced into a flask connected to a condenser containingalcohol at -20°C, stirred and heated to 120°C in an oil bath, added alkyl borate dropwise during 10 min, stirred for further 20 min; distd.; gas chromy.;
参考文献
Journal of Organometallic Chemistry, , vol. 317, p. 277 - 284
in neat (no solvent) Sonication; (N2), Et3Al*Et2O introduced into a flask connected to a condenser containing alcohol at -20°C, stirred and heated to 120°C in an oil bath, added alkyl borate dropwise during 10 min, stirred for further20 min; distd.; gas chromy.;
参考文献
Journal of Organometallic Chemistry, , vol. 317, p. 277 - 284