反应详情

A solution of 2-fluorobenzonitrile (2.75 g, 22.7 mmol) and 4-piperidone ethylene ketal (4.25 g, 29.7 mmol) in DMF (40 mL) was heated to 120° C. for 4 h. The resulting mixture was cooled to room temperature overnight. The solvent was removed in vacuo and the residue dissolved in ether and sodium bicarbonate solution. The aqueous layer was extracted with two additional portions of ether and the combined organic extracts were washed with brine, dried over Na2SO4, and concentrated under reduced pressure to afford the title compound (4). The crude product was used directly.

1. customThe solvent was removed in vacuo
2. dissolutionthe residue dissolved in ether
3. extractionThe aqueous layer was extracted with two additional portions of ether
4. washthe combined organic extracts were washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure