in decalin byproducts: CO; 3.5:1 mixture of arene and Cr(CO)6 in solvent purged for 20 min with Ar, evacuated for 20 min, mixture refluxed, cooled to 20°C, cooled to -18°C under argon, reaction time 5.5 h; filtered off, dissolved in benzene, filtered through Kieselguhr, concentrated, light petroleum added, crystn. at -18°C, complexes eluted with benzene/ethyl acetate, elem. anal., NMR;

trifluoroacetic acid in tetrahydrofuran addn. of known excess of Et3BHLi to N,N-dimethylaminoarenetricarbonylchromium (THF, room temp.), stirring (several h, N2), addn. to a soln. of CF3CO2H (THF, excess); extn., neutralization, sepn. (silica gel flash chromy.), recrystn. (acetone/light petroleum);

carbon monoxide in neat (no solvent) in autoclave at 270-300°C, 28 atm CO pressure;;

in tetrahydrofuran N2-atmosphere; refluxing (1 d);

in neat (no solvent) in bomb tube at 160-170°C;;

in neat (no solvent) in bomb tube at 160-170°C;;

in 1,4-dioxane refluxed for 5 h under N2; filtrate concd., chromy. (alumina);

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Yield given. Multistep reaction;

Yield given. Multistep reaction;