Trichlorotris(tetrahydrofuran)molybdenum(III) (MoCl3(THF)3), is a widely used starting material for the synthesis of a broad range of molybdenum compounds. It was first prepared by a carbonyl route, but later the compound was obtained by a reductive procedure in three steps starting from MoCl5. In spite of the various incremental improvements, the three-step procedure remains rather long and requires isolation of both the MoCl4(MeCN)2 and MoCl4(THF)2 intermediates in order to obtain product of sufficient quality. Ethereal solutions of MoCl5 are stable and their conversion to tetrachlorobis(diethyl ether)molybdenum(IV) (MoCl4(OEt2)2) by reducing agents such as norbornene or allyltrimethylsilane has been previously reported. As it turns out, this reduction can be conveniently carried out by metallic tin. This chapter describes both the synthesis and isolation of the MoCl4(OEt2)2 complex and the direct, two-step, single-flask synthesis of MoCl3(THF)3 from MoCl5.