反应详情

Iron powder (16.4 g, 294 mmol) was slowly added to an ice-cold solution of 1-(2-fluoro-4-nitro-phenyl)-piperidin-4-one (7 g, 29.4 mmol), obtained in Preparation 5, in ethanolic HCl (50 ml) at 0° C. and stirred at the same temperature for 2 h. The reaction mixture was basified by the addition of sodium carbonate and pH of the solution was brought to 8. It was then diluted with ethyl acetate (100 ml) and the aqueous layer was separated. The aqueous layer was further extracted with ethyl acetate (100 ml×2). Combined organic extract was washed with water followed by brine and dried over sodium sulfate. Removal of volatiles left a pasty mass (7 g), which was used for the next step.

1. customthe aqueous layer was separated
2. extractionThe aqueous layer was further extracted with ethyl acetate (100 ml×2)
3. extractionCombined organic extract
4. washwas washed with water
5. dry with materialdried over sodium sulfate
6. customRemoval of volatiles
7. waitleft a pasty mass (7 g), which