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NbBr4 thf

A dry three-necked 1-L flask is fitted with an overhead mechanical stirrer, an addition funnel, and a nitrogen inlet adapter and charged with toluene (600 mL) and NbBrj (40.0 g, 81.2 mmol). The addition funnel is charged with tetrahydrofuran (120 mL, 1.48 mol) and tributyltin hydride (23.6 g, 81.1 mmol). The reaction is cooled using an ice bath and the solution is [Pg.121]

Stirred vigorously while the tributyltin hydride solution is added over 0.5 h. After the addition is completed, the mixture is stirred an additional 45 min and then filtered. The solid is washed with toluene (2 x 150 mL) and pentane (2 X 150 mL) and dried in vacuo (6 h, 1 mm) to give 36.3 g (80%) of a red-orange powder. Melting point (sealed capillary) = 97°C dec. IR (cm , Nujol mull) V 990, 816. [Pg.122]

The checkers analyzed for niobium. Calcd. Nb, 16.69. Found Nb, 16.9. [Pg.122]

The product has been previously prepared by reaction of NbBr with tetrahydrofuran. This complex must be stored in a low temperature freezer ( -30 C). [Pg.122]

A three-necked I-L flask is fitted with an overhead mechanical stirrer and a nitrogen inlet adapter and charged with dry 1,2-dimethoxyethane (600 mL) and tributyltin hydride (59.0 g, 0.203 mol). A 250-mL flask containing niobium pentabromide (50.0 g, 0.102 mol) is attached to the setup via a piece of Latex tubing (30 cm long, 1.8 cm in diameter) that is adapted with two male 24/40 joints on each end. The reaction mixture is cooled to — 78°C (Dry lce/2-propanol) and the solution is stirred vigorously while the NbBtj is added in portions over a 30-min period.t [Pg.122]


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