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Sodium nitrite (9.9 g, 144 mmol) was added to an ice-cooled solution of 1-(4-amino-2-fluoro-phenyl)-piperidin-4-one (15 g, 72 mmol), obtained in Preparation 10, in 6 N HCl (60 ml) and the resulting solution was stirred at 0° C. for 0.5 h. An aqueous solution of sodium azide (9.4 g, 144 mmol) and sodium acetate (118 g, 1.44 mol) was then added. The reaction mixture was extracted with ethyl acetate (100 ml×2) and the combined extracts were washed with 5% sodium bicarbonate solution followed by brine and dried over sodium sulfate. Removal of volatiles left a crude product, which was purified by silica gel column chromatography (ethyl acetate/pet. ether, 1:1) to obtain the title azide (10 g, 63%).

1. extractionThe reaction mixture was extracted with ethyl acetate (100 ml×2)
2. washthe combined extracts were washed with 5% sodium bicarbonate solution
3. dry with materialdried over sodium sulfate
4. customRemoval of volatiles
5. waitleft a crude product, which
6. customwas purified by silica gel column chromatography (ethyl acetate/pet. ether, 1:1)