Swivel frit assembly

Figure 3. High vacuum line work station with solvent pot (left) and swivel frit assembly (right).

Adding Reagents to the Reaction Flask of the Swivel Frit Assembly... 

A sample of 83 (0.35 g, 0.94 mmol) and benzene (10 ml) were placed in a round-bottomed flask attached to a swivel-frit assembly. The soln was stirred under N2O (1 atm) at 55 °C for 3 d, after which the soln was filtered and the filtrate was taken to diyness under vacuum. The resulting solid was washed with petroleum ether (3x5 mL), and the blue product was collected on a filter frit to give microcrystalline 84 jdeld 0.16 g (44%). 

In a dinitrogen-filled glove box, 1 (0.420 g, 1.2 mmol) and ortAo-tolyllithium (0.18 g, 1.8 mmol) are transferred to a 50 mL round-bottomed flask fitted with a swivel frit assembly. The reaction mixture is stirred for 12 h at room temperature, and the volatile materials are removed under reduce pressure. Petroleum ether (10 mL) is transferred onto the solid in vacuum, and the resulting solution is filtered to remove LiCl. The residue is washed with additional pentane (2 X10 mL) using standard swivel frit techniques. The filtered washings are combined, concentrated to 3 mL, and cooled to —78°C. The resulting off-white precipitate is isolated by cold filtration. Yield 0.285 g (59%). 

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