in acetic acid byproducts: CO; other Radiation; addn. of molybdenum compd. to acetic acid, irradiation with stirring in closed vessel for 10 min at 300 W in microvawe reactor, cooling to 54°C, venting, irradiation of additional 6 min; cooling to room temp., filtration, washing with ethanol, hexane and diethyl ether, drying in vac. desiccator, elem. anal.;

NaBr; (CH3CO)2O in acetic acid refluxing for 12 h in an inert atmosphere; cooling, filtn. of Mo(O2CCH3)4, addn. of H2O, stirring (1 h), passing of soln. through a Dowex 50W x 2 column, washing with aq. oxalic acid and aq. HClO4, washing with H2O, elution with aq. HClO4;

acetic anhydride in acetic acid in a microwave oven (Fischer-Porter reaction vessel) at 195°C for 30 min; elem. anal.;

acetic anhydride in acetic acid acetic acid and acetic anhydride added to Mo2Br4(CO)8 at -40°C under Ar, mixt. stirred, left to warm to room temp. overnight, refluxed 4h; slowly cooled to room temp., pptn.; concn. of mixt. to 1/4 of initial volume, filtered, washed (benzene), dried (vac.);

in acetonitrile inert atmosphere; large excess of acid/anhydride;

HCl or CF3CO2H in water; acetic anhydride; acetic acid mixt. of Mo-complex, CH3CO2H and (CH3CO)2O refluxed for 12 h under N2, cooled to room temp., filtered in air, filtrate diluted with H2O, pouredon cation-exchange column (0.1 M HCl or CF3CO2H), evapd. to dryness on rotary evaporator; further reagents; dissolved in MeOH, passed through Dowex column, eluted with 0.1 M NaSbF6 soln. in MeOH, evapd. slowly in air;

acetic acid; acetic acid anhydride; KMnO4 in water; acetic anhydride; acetic acid mixt. of Mo-complex, CH3CO2H and (CH3CO)2O refluxed for about 12 h under N2, cooled to room temp., filtered in air, filtrate diluted with H2O, poured on cation-exchange column (0.1 M HCl), 0.1 M KMnO4 soln. added slowly dropwise; further reagents; poured on Dowex column, washed with 0.1 M HCl, eluted with 1 M soln. ofCF3SO3H, evapd. slowly in air; elem. anal.;

acetic acid; acetic acid anhydride; KMnO4 in water; acetic anhydride; acetic acid mixt. of Mo-complex, CH3CO2H and (CH3CO)2O refluxed for about 12 h under N2, cooled to room temp., filtered in air, filtrate diluted with H2O, poured on cation-exchange column (0.1 M HCl), 0.1 M KMnO4 soln. added slowly dropwise; further reagents; poured on Dowex column, washed with 0.1 M HCl, eluted with 0.5 M soln. of p-CH3C6H4SO3H, evapd. slowly in air; elem. anal.;

in tetrahydrofuran N2-atmosphere; equimolar amts., stirring for 1 h; filtration, solvent removal;

in tetrahydrofuran N2-atmosphere; excess AcOH, stirring for 1 h; filtration, solvent removal;