In order to develop an alternative preparation method of uranium(III) precursors soluble in aprotic organic solvent used for the preparation of uranium(III) compounds, U(IV) triflate, U(OTf) 4, in tetrahydrofuran (THF) was reduced to produce uranium(III) triflate. U(OTf)4 in THF was completely reduced by large excess of zinc within 25 minutes. Energies and molar coefficients of the absorption bands of U(III) triflate are close to those of U(III) in 1M HCl aqueous solution especially in the range of (9 ∼ 14)×10 3 cm −1 . U(III) triflate solution maintains its oxidation state in THF is when it is contacted with zinc amalgam for more than a week.