aluminium trichloride; ethylmagnesium bromide in diethyl ether Bu3SnCH(OEt)2 reacted with 20percent excess of (PhCC)(n)AlX(3-n) obtained from exchange between Grignard reagent (obtained conventionally from PhCCH and EtMgBr) and AlCl3 in Et2O at 20°C;

in not given byproducts: ethyl acetate; excess of acetyl chloride added to Bu3SnCH(OEt)2 under N2, stirred at room temp. for 1.5 h, volatiles removed in vacuo; identified by NMR spectra;

n-butyllithium in tetrahydrofuran; hexane 1.) -78 deg C; 2.) up to 0 deg C;

water; ammonium chloride in diethyl ether byproducts: tetrabutyltin, hexabutyltin, tributyltin acetate; dropwise addn. of diethoxymethylacetate (0.485 mol, 1:1 mixt. with ether) to soln. of (C4H9)3SnMgCl (0.5 mol) in ether under N2 at 0°C during 1 h; stirring for 1 h; hydrolysis with H2O/NH4Cl;; filtering, decanting and drying over MgSO4; removing ether under vac.; flash chromy. of residue on silica gel (eluent: hexane/ether/triethylamine); removing solvents; determination of purity by gas-liquid-chromy. analysis;;

in diethyl ether grignard reagent in Et2O adding to Sn hydride soln. in Et2O, resulting Bu3SnMgCl adding dropwise to orthoformate in Et2O, stirring for 3 h, hydrolyzing, org. phase sepg.; purified by distn. in vacuo; NMR, IR and mass spectra;

byproducts: CH3CH2OMgCl; Sn compd. treated with org. compd.;

byproducts: C6H5OMgCl; Sn compd. treated with org. compd.; distillation;

aluminium in diethyl ether Bu3SnCH(OEt)2 reacted with 20percent excess of (CH2CHCH2)(n)AlBr(3-n) (obtained from CH2CHCH2Br and Al) in Et2O at 35°C;

n-butyllithium in tetrahydrofuran; hexane 1.) -78 deg C; 2.) up to 0 deg C; Yield given. Yields of byproduct given;

n-butyllithium 1.) THF, -78 deg C, 2.) THF; Yield given. Multistep reaction;