in tetrahydrofuran 8 ml THF was condensed onto a solid mixture of {{C5H5(CO)Fe}2(μ-CO)(μ-CHCO)}PF6 and Et4N{HFe(CO)4} at -78°C, stirred at -78°C for 90 min, evapn. of solvent, residue extracted into CH2Cl2;; chromy. (Al2O3, hexane/Et2O=1:1) giving {C5H5(CO)Fe}2(CO)(CH2), chromy. (acetone/Et2O=1:1) giving mixt. of NEt4PF6 and {C5H5(CO)Fe}2(CO)(CHCHO), extn. into Et2O, filtration through Celite, evapn., washing with hexane, drying, elem. anal.;;

in acetonitrile T=-30°C; 12 h;

in N,N-dimethyl-formamide; acetonitrile byproducts: sulfur; oxomolybdate dissolved in CH3CN, addn. (2-3 min) of ferrocenium dissolved in DMF, stirring (5 min), concn. (-196°C, 0.1 Torr), filtration in vac., addn. of propanol, keeping at 0°C (12 h); filtration, washing (diethyl ether), recrystn. (MeCN/2-propanol) at 0°C; elem. anal., powder X-ray diffraction;

T=20°C;

in further solvent(s) in liq. H2S at -78°C;

1: ethanol / 12 h / 80 °C / |Inert atmosphere 2: 20 °C View Scheme

HPF6; sodium hydroxide

Petroleum ether durch Zerlegung des entstandenen Aethylsulfats mit wss. Ba(OH)2;