in toluene byproducts: HCl; at -78°C for 1 h, warm to room temp. refluxed at reduced press. at 70°C for 36 h; solvent removed under vac., recrystn. from toluene/hexane or by very short-path distn. or sublimation under high vac., elem. anal.;

in toluene byproducts: HCl; at -78°C for 1 h, warm to room temp. refluxed under atm. press. of N2 for 1 week, product dissolved in toluene, addn. of hexane; solvent removed under vac., recrystn. from hexane, elem. anal.;