反应详情

温度

5 °C

12.4 g 1-Dimethylamino-piperidin-4-one oxime (from Step 1) is dissolved in 160 ml water. 49.3 g potassium dihydrogenphosphate is added. The resulting yellow suspension is cooled to 5° C., and a solution of 11.24 g potassium cyanide in 40 ml water is added. The mixture is stirred at room temperature for 2 days, then extracted with ethyl acetate, the organic layer dried over sodium sulfate, and the solvent evaporated, to give 7.8 g 1-Dimethylamino-4-hydroxyamino-piperidine-4-carbonitrile. 1H-NMR (CDCl3): 5.60 ppm (s, broad, 1H), 5.10 ppm (s, broad, 1H), 2.92 ppm (m, 2H), 2.61 ppm (m, 2H), 2.33 ppm (s, 6H), 2.10 ppm (m, 2H), 1.70 ppm (m, 2H).

1. extractionextracted with ethyl acetate
2. dry with materialthe organic layer dried over sodium sulfate
3. customthe solvent evaporated