Reaction between tetramethylammonium fluoride (CH3)(4)NF and MoO3 in 1:1 mo
lar ratio in the minimum amount of dry acetonitrile gives tetramethylammoni
um trioxyfluoromolybdate (VI), (CH3)(4)N[MoO3F] in very high yields. The co
mpound has been characterized by elemental analyses and IR spectral studies
. The advantages of the new method are discussed.