thionyl chloride from 0 deg C up to room temp.; reflux, 30 min;

in not given dropwise addn. of thionyl chloride to tetraalkyltin(IV) compd. under dry N2 atmosphere under ice cooling, warming to room temp., refluxing for 30 min; distn. (removal of excess of SOCl2), cooling resulting liquids, sepn., elem. anal.;

triethylamine; zinc in triethylamine 160°C;

zinc in tetrahydrofuran; water under air atm., at room temp., cosolvent media: H2O(NH4Cl)/THF/Zn, alkyliodide was added dropwise to the alkyl tin halide in solvent mixt. over 15 min, reaction time: 1.0 h, (H2O/THF=100/50); Zn was filtered off, aq. phase was extd. three times with n-pentane, organic phase was washed with sat. aq. NaCl and dried over MgSO4, solvent was removed, crude oil was distilled under vac.; (119Sn NMR monitoring);

in diethyl ether; benzene boiling for 3h, addn. of aq. NH4Cl;;

copper; zinc at 80°C, 2h;;

in toluene at 80°C, excess Al(C2H5)3;;

in tetrahydrofuran boiling, 4.5h;;

暂无反应条件数据

triethylamine; zinc in mixture with other products, GC;;