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