triethyl borane in mineral oil addn. of a small amount of B(C2H5)3 and N(C2H5)3 to NaH in mineral oil at 70°C, addn. of BCl3 at 70-80°C while stirring;; separation by distn.;;
in dichloromethane all reactions under Ar atm.; soln. of BCl3 in CH2Cl2 added to stirred soln. of triarylstibane at 0°C, stirred for 2 h, allowed to warm toroom temp., solvent removed in vac., oil dissolved in MeOH, stirred for 30 min at room temp., diol added; stirred for 1 h, solvent removed in vac., chromy. (silica-gel, hexane/CH2Cl2);
in dichloromethane all reactions under Ar atm.; soln. of BCl3 in CH2Cl2 added to stirred soln. of triarylstibane at 0°C, stirred for 2 h, allowed to warm toroom temp., solvent removed in vac., oil dissolved in MeOH, stirred for 30 min at room temp., diol added; stirred for 1 h, solvent removed in vac., chromy. (silica-gel, hexane/CH2Cl2);
in dichloromethane all reactions under Ar atm.; soln. of BCl3 in CH2Cl2 added to stirred soln. of triarylstibane at 0°C, stirred for 2 h, allowed to warm toroom temp., solvent removed in vac., oil dissolved in MeOH, stirred for 30 min at room temp., diol added; stirred for 1 h, solvent removed in vac., chromy. (silica-gel, hexane/CH2Cl2);
in dichloromethane all reactions under Ar atm.; soln. of BCl3 in CH2Cl2 added to stirred soln. of triarylstibane at 0°C, stirred for 2 h, allowed to warm toroom temp., solvent removed in vac., oil dissolved in MeOH, stirred for 30 min at room temp., diol added; stirred for 1 h, solvent removed in vac., chromy. (silica-gel, hexane/CH2Cl2);
in dichloromethane all reactions under Ar atm.; soln. of BCl3 in CH2Cl2 added to stirred soln. of triarylstibane at 0°C, stirred for 2 h, allowed to warm toroom temp., solvent removed in vac., oil dissolved in MeOH, stirred for 30 min at room temp., diol added; stirred for 1 h, solvent removed in vac., chromy. (silica-gel, hexane/CH2Cl2);
in dichloromethane all reactions under Ar atm.; soln. of BCl3 in CH2Cl2 added to stirred soln. of triarylstibane at 0°C, stirred for 2 h, allowed to warm toroom temp., solvent removed in vac., oil dissolved in MeOH, stirred for 30 min at room temp., diol added; stirred for 1 h, solvent removed in vac., chromy. (silica-gel, hexane/CH2Cl2);
in dichloromethane all reactions under Ar atm.; soln. of BCl3 in CH2Cl2 added to stirred soln. of triarylstibane at 0°C, stirred for 2 h, allowed to warm toroom temp., solvent removed in vac., oil dissolved in MeOH, stirred for 30 min at room temp., diol added; stirred for 1 h, solvent removed in vac., chromy. (silica-gel, hexane/CH2Cl2);