Reaction between tetramethylammonium fluoride (CH3)(4)NF and CrO3 in 1:1 mo
lar ratio in the minimum amount of dry acetonitrile gives tetramethylammoni
um trioxyfluorochromate(VI), (CH3)(4)NCrO3F in very high yields. The compou
nd has been characterized by elemental analyses and IR spectral studies. Th
e advantages of the new method are discussed.