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: 4.5 h; 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., then chromd. using n-hexane; (119Sn NMR monitoring);

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: 5.0 h, after 1.5 h a further addition of alkyl i odide was carried out; 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., then chromd. using n-hexane; (119Sn NMR monitoring);

Zn; NH4Cl in tetrahydrofuran; water

in diethyl ether stirred for 1h; treated with 10percent NH4Cl soln., extracted twice with Et2O, chromy. (Fluorisil/hexane); elem. anal.;

aluminium trichloride 119-200°C, 2.5 Torr;;

1: C4H9Cl 2: AlCl3 View Scheme

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