反应详情

Ethyl 1-benzyl-5,5-difluoro-4-oxopiperidine-3-carboxylate (6.00 g, 20.2 mmol; prepared as described in WO 2005/040120, p. 30) was dissolved in 3N HCl (60 mL) and heated to reflux for 16 hours. The reaction was cooled, adjusted to pH 8 with solid NaHCO3, then extracted three times with ethyl acetate. The combined organics were washed with saturated NaCl, dried over Na2SO4 and concentrated in vacuo to a white solid (5.1 g). MS APCI (+) m/z 244.0 (M+1) detected.

1. temperatureheated
2. temperatureto reflux for 16 hours
3. temperatureThe reaction was cooled
4. extractionextracted three times with ethyl acetate
5. washThe combined organics were washed with saturated NaCl
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo to a white solid (5.1 g)