HCl in benzene HCl gas, at room temp, under Ar in the dark; elem. anal.;

in chloroform byproducts: C6H6; (Ar); standard Schlenk technique; stirred suspn. of Pb compd. in CHCl3 was treated with stream of HCl for 2 h; filtered; washed (CHCl3);

in methanol 2 h;

in chloroform to refluxing soln. of Ph2Pb2 in chloroform is added dropwise chloroformsoln. of (C6F5)3SbCl2 and mixt. is refluxed for 5 h; mixt. is cooled at ice temp., solid is filtered off;

in tetrahydrofuran byproducts: NaCl, PbS; addn. of Pb compd. in portions to Na2S suspension under N2, room temp., 30 min; pptn.; stirring, room temp., 14h; pouring into water; filtration; extn. of ppt. with ether; evapn.; drying (vac., 30 min); recrystn. (benzene, hexane); elem. anal.;

in not given byproducts: Pb, LiCl; inert atmosphere;

in diethyl ether byproducts: LiCl; all manipulations under N2 atm.; soln. of Pb compd. added dropwise to suspn. of Fe compd. at -78°C with stirring, stirred for 2.5 h at this temp. in dark, allowed to warm to room temp.; filtered in cold, solvent removed, by recrystallization at room temp. obtained Pb and Fe compd., purification of Fe-Pb compd. by recrystn. at -30°C proved unsuccesful;

in methanol byproducts: AgCl; Pb compd. reacted with Ag salt in MeOH;

暂无反应条件数据

Et3N in diethyl ether byproducts: Et3NHCl; Schlenk technique, N2; Pb-compd. addn. to dithiol soln., Et3N soln. addn. dropwise, mixt. stirring at room temp. 18 h in flask wrapped with Al foil, filtration, solvent removal, ppt. treatment with H2O, residue dissoln. (CH2Cl2/CH3CN), drying (Na2SO4); soln. filtration, solvent removal; elem. anal.;