True nature of trihalotris(tetrahydrofuran)molybdenum(III), MoX3(THF)3 (X = Cl, Br, I). A paramagnetic proton NMR study

Abstract

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Improved Preparations of Molybdenum Coordination Compounds from Tetrachlorobis(diethyl ether)molybdenum(IV)

“…C 34.43, H 5.78; found C 34.04, H 5.51. The 1 H NMR properties of this material correspond with those previously described for [MoCl 3 (THF) 3 ] 34…”

Alkyne Metathesis: Development of a Novel Molybdenum-Based Catalyst System and Its Application to the Total Synthesis of Epothilone A and C

“…These were prepared by reaction of [MoCl 3 (thf) 3 ] with the lithium salt of a suitable secondary amine ( t Bu)(Ar)NH under carefully controlled reaction conditions 26, 27. While the access to [MoCl 3 (thf) 3 ] is fairly routine and well described in the literature,28 a high yielding and flexible entry into the required bulky amines was crucial. The palladium catalyzed amination of aryl halides turned out to be the method of choice 29, 30.…”

“…[MoCl 4 (thf) 2 ] :28 MoCl 5 (6.37 g, 23.3 mmol) was added to acetonitrile (32 mL) and the resulting mixture was stirred for 3 h at ambient temperature. The suspension was filtered, the solid residue was washed with CH 3 CN (15 mL) and dried in vacuo, affording [MoCl 4 (CH 3 CN) 2 ] as a brown powder (5.9 g, 80 %).…”

“…[MoCl 3 (thf) 3 ] :28 Sn shots (7.1 g, 59.8 mmol) were added to a suspension of [MoCl 4 (thf) 2 ] (3.55 g, 9.3 mmol) in THF (43 mL). While the resulting suspension was vigorously stirred for 30 min, a color change from orange to orange‐green was observed.…”

Ether Complexes of Molybdenum(III) and Molybdenum(IV) chlorides

“…It is a beige crystalline product that deteriorates upon exposure to the laboratory atmosphere and progressively transforms to darker dinuclear complexes upon partial loss of THF ([Mo2Cl6(THF)4] and [Mo2Cl6(THF)3]) when dissolved or suspended in solvents other than THF. 9 It also decomposes slowly in THF, especially upon warming, with formation of 1,4 dichlorobutane and more soluble oxo derivatives whose precise nature is unknown. Therefore, it is important to avoid to leave the compound in THF for a long time in order to obtain a good yield.…”