in acetone -70°C, several hours, warming to room temp.; redn. of vol. (distn., vac., room temp.), pptn. on addn. of water, crystn. (overnight), dissolving (acetone), pptn. on pentane addn., crystn. (several days);

in diethyl ether under N2 atm. to soln. (Fe(CO)5) in Et2O LDA was added dropwise, react.was cooled (dry ice/propanone) and (CF3CO)2O in Et2O was added and mixt. was stirred at low temp. for 15 min, PPh3 was added and react. was allowed to warm to room temp. overnight; react. was cooled to room temp., soln. was filtered, solvent was removed under reduced pressure, residue was extd. with mixt. propanone and light petroleum, extracts were concd. and cooled, crystals were dried in vacuo; elem. anal.;

in diethyl ether under N2 atm. to soln. (Fe(CO)5) in Et2O LDA was added dropwise, react.was cooled (dry ice/propanone) and (CF3CO)2O in Et2O was added and mixt. was stirred at low temp. for 90 min, PPh3 was added and react. was allowed to warm to room temp. overnight; react. was cooled to room temp., ppt. was separated, CF3COOLi was removed by extn. with mixt. dichloromethane and light petroleum and filtration, product was purified by chromy.; elem. anal.;

in diethyl ether addn. of Ag(CF3CO2) at -78°C to a soln. of Li(C6F5) in diethyl ether, stirred for 60 min under N2, addn. of (PPh3CH3)(CF3CO2), stirred for 10 min, warmed to room temp.; pptn. filtered off, washed with water, dissolved in diethyl ether, filtered through a layer of anhydrous MgSO4, evapn., addn. of n-hexane, pptn.; elem. anal.;

in diethyl ether addn. of Ag(CF3CO2) to a soln. of Li(C6F5) in diethyl ether at -78°C, stirred for 60 min under N2, addn. of (P(C6H5)2(CH3)2)(CF3CO2), stirred for 10 min, warmed to room temp.; filtered, concd., addn. of n-hexane, recrystn.; elem. anal.;

in diethyl ether addn. of Ag(CF3CO2) to a soln. of Li(C6F5) in diethyl ether at -78°C, stirred for 60 min, warmed to 0°C, addn. of three drops of water, stirred for 15 min, addn. of (AsPh3Me)(CF3CO2), warmed to room temp., stirred for 45 min; evapd. to dryness, residue washed with water, extn. (diethyl ether), filtered through a layer of anhydrous MgSO4, evapn., addn. of n-hexane; elem. anal.;

in diethyl ether addn. of Ag(CF3CO2) to a soln. of Li(C6F5) in diethyl ether at -78°C, stirred for 60 min under N2, addn. of (As(C6H5)3CH3)(CF3CO2), stirred for 10 min, warmed to room temp.; pptn. filtered off, washed with water, dissolved in diethyl ether, filtered through a layer of anhydrous MgSO4, evapd., addn. of n-hexane, pptn.; elem. anal.;

in diethyl ether addn. of Ag(CF3CO2) to a soln. of Li(C6F5) in diethyl ether at -78°C, stirred for 60 min under N2, addn. of (P(C6H5)(CH3)3)(CF3CO2), stirred for 10 min, warmed to room temp.; pptn. filtered off, washed with water, dissolved in diethyl ether, filtered through a layer of anhydrous MgSO4, evapd., addn. of n-hexane, pptn.; elem. anal.;

trifluoroacetic acid in acetone byproducts: I2; -70°C; pptn. on warming to room temp.;

in not given noncrystallizable oil;